CPC

Concurrent

Technologies

Corporation

U.S. Environmental Protection Agency

Environmental Technology Verification Program

For Metal Finishing Pollution Prevention Technologies

Verification Test Plan

for the

Evaluation of The MART Corporation's EQ-1™
Wastewater Processing System

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.

Revision 0

January 5,2001


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ElV

Concurrent
CfC	Technologies

Corporation

U.S. Environmental Protection Agency
Environmental Technology Verification Program
For Metal Finishing Pollution Prevention Technologies

Verification Test Plan

for the

Evaluation of The MART Corporation's EQ-1™
Wastewater Processing System

January 5,2001

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TITLE:	EVALUATION OF THE MART CORPORATION'S EQ-11

WASTEWATER PROCESSING SYSTEM

ISSUE DATE: January 5, 2001

DOCUMENT CONTROL

This document will be maintained by Concurrent Technologies Corporation (CTC) in accordance
with the EPA Environmental Technology Verification Program Quality and Management Plan
for the Period 1995-2000 (EPA/600/R-98/064). 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 Kanie Jethrow, Percy Peltzer, Jim Totter, Scott Maurer and Valerie
Whitman 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.

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Environmental Technology Verification for Metal Finishing Pollution Prevention Technologies
Program: Verification Test Plan for the Evaluation of MART Corporation's EQ-1™ Wastewater
Processing System.

Prepared By:

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Troy Cramer, Ohio Air National Guard
Base Environmental Manager — 179th Airlift Wing

/ _ / 
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TABLE OF CONTENTS
1.0 INTRODUCTION	1

1.1 Background	2

2.0 TECHNOLOGY DESCRIPTION	2

2.1	Theory of Operation	2

2.2	Commercial Status	4

2.3	Pollution Prevention Classification	4

2.4	Environmental Significance	4

3.0 PROCESS DESCRIPTION	4

3.1	Equipment and Flow Diagram	4

3.2	Testing Site	5

3.3	The 179th AW C-130H Engine Cleaning Process	7

3.4	The 179th AW Parts Washer Cleaning Process	8

4.0 EXPERIMENTAL DESIGN	9

4.1	Test Goals and Objectives	9

4.2	Critical and Non-Critical Measurements	10

4.3	Test Matrix	10

4.3.1	Engine Spent Cleaning Wash Wastewater - Test #1	12

4.3.2	Parts Washers' Wastewater - Test #2-4	12

4.4	Testing and Operating Procedures	12

4.4.1	Set-Up and System Initialization Procedures	12

4.4.2	System Operation	13

4.4.3	Sampling and Process Measurements	14

4.4.3.1	Sampling Responsibilities & Procedures	14

4.4.3.2	Process Measurements	16

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4.4.3.2.1 Calibration Procedures and Frequency	16

4.5	T esting Parameters	17

4.5.1	Oil/Grease Concentration	17

4.5.2	Cleaner Concentration	17

4.5.3	Metals	18

4.5.4	Total Suspended Solids	19

4.6	Air Monitoring	19

5.0 QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS	20

5.1	Quality Assurance Obj ectives	20

5.2	Data Reduction, Validation, and Reporting	20

5.2.1	Internal Quality Control Checks	20

5.2.2	QA/QC Requirements	21

5.2.2.1	Duplicates	21

5.2.2.2	Matrix Spikes	22

5.2.2.3	Field Blanks	22

5.2.3	Calculation of Data Quality Indicators	22

5.2.3.1	Precision	24

5.2.3.2	Accuracy	24

5.2.3.3	Comparability	25

5.2.3.4	Completeness	25

5.2.3.5	Representativeness	25

5.2.3.6	Sensitivity	26

5.2.4	Mass Balance	26

5.2.4.1	Cleaner Recovery Efficiency	28

5.2.4.2	Oil Removal Efficiency	28

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5.2.4.3 Cadmium Removal Efficiency	28

5.2.5	Energy Use	28

5.2.6	Cost Analysis 	29

5.2.7	Waste Generation Analysis	29

5.3 Quality Audits	29

6.0 PROJECT MANAGEMENT	30

6.1	Organization/Personnel Responsibilities	30

6.2	Test Plan Modifications	30

7.0 UTILITY REQUIREMENTS	31

8.0 HEALTH AND SAFETY PLAN	31

8.1	Hazard Communication	31

8.2	Emergency Response Plan	31

8.3	Hazard Controls Including Personal Protective Equipment	31

8.4	Lockout/Tag out Program	31

8.5	Material Storage	32

8.6	Safe Handling Procedures	32

9.0 WASTE MANAGEMENT	32

10.0 TRAINING	32

11.0 REFERENCES	33

12.0 DISTRIBUTION	33

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LIST OF APPENDICES

APPENDIX A: The 179th AW Cleaner MSDSs	A-1

APPENDIX B: The MART EQ-1™ System O&M Manual	B-1

APPENDIX C: Test Plan Modification Request	C-1

APPENDIX D: ETV-MF Operation Planning Checklist	D-1

APPENDIX E: Job Training Analysis Form	E-1

APPENDIX F: ETV-MF Proj ect Training Attendance Form	F-1

LIST OF FIGURES

Figure 1: The MART EQ-1™ Unit	3

Figur e 2: The MART EQ -1 ™ S chemati c	6

Figure 3: The 179th AW Wash Wastewater Collection Container	8

Figure 4: Data Collection Form	15

Figure 5: Fundamental Material Balance Equation	27

Figure 6: Material Balance Equation for MART'S System	27

LIST OF TABLES

Table 1: Untreated Engine Wash Wastewater Background Analysis	8

Table 2: Parts Washers at the 179th AW	9

Table 3: Test Objectives and Related Test Measurements for Evaluation of the MART
EQ-1™	11

Table 4:	Magic Dust Addition to Wastewater	13

Table 5:	Sampling Frequency and Parameters to Be Measured	14

Table 6:	Summary of Analytical Tests and Requirements	18

Table 7:	QA Objectives for Precision, Accuracy, and Detection Limits	23

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ACRONYMS & ABBREVIATIONS

AGE

Aircraft Ground Equipment

VIIIA

American Industrial Hygiene Association

ANG

Air National Guard

AW

Airlift Wing

Ba

Barium

C-130H

C-130 Hercules

CAS#

Chemical Abstract Number

Cd

Cadmium

Cr

Chromium

CTC

Concurrent Technologies Corporation

Cu

Copper

DOD

Department of Development

EPA

Environmental Protection Agency

ETV-MF

Environmental Technology Verification for Metal Finishing Pollution Prevention



Technologies

IPS

Final Polishing System

ft3

Cubic feet

g/L

Grams per liter

gph

Gallon per hour

gpm

Gallon per minute

Hcl

Hydrochloric acid

HP

Horsepower

HQ

Headquarters

hr

Hour

Hz

Hertz

ID

Identification

IDL

Instrument detection limit

JTA

Job Training Analysis

kWh

Kilowatt hour

lb.

Pound

L

Liter

Lpm

Liter per minute

MART

The MART Corporation

MDL

Method detection limit

ml

Milliliter

mm

Millimeter

MRL

Method reporting limit

MSDS

Material Data Safety Sheet

Ni

Nickel

NIOSH

National Institute of Occupational Safety and Health

O&G

Oil and Grease

O&M

Operation and Maintenance

OSIIA

Occupational Safety and Health Administration

PARCCS

Precision, Accuracy, Representativeness, Comparability, Completeness, and

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Sensitivity

Pb

Lead

POTW

Publicly Owned Treatment Works

PPE

Personal Protection Equipment

PPi"

Part per million

PQL

Practical quantification limit

psi

Pounds per square inch

PVC

Polyvinyl chloride

QA

Quality Assurance

QC

Quality Control

QMP

Quality Management Plan

Ref.

Reference

RPD

Relative Percent Difference

rpm

Revolutions per minute

SM

Standard Methods for Examination of Water and Wastewater, 20th ed (1998)

SOP

Standard Operating Procedures

STEL

Short Term Exposure Limit

TCLP

Toxicity Characteristic Leaching Procedure

TPH

Total Petroleum Hydrocarbons

TS

Total solids

TSS

Total suspended solids

TWA

Time weighted average

U.S.

United States

VAC

Vacuum



Micron

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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 the Ohio Air National Guard (ANG) 179th Airlift Wing
(AW), during verification testing of The MART Corporation's EQ-1™ Wastewater Processing
System. This test plan has been prepared to evaluate the performance of the technology by the
U.S. Environmental Protection Agency's (EPA's) Environmental Technology Verification for
Metal Finishing Pollution Prevention Technologies (ETV-MF) Program. The objective of this
program is to identify promising and innovative pollution prevention technologies through EPA-
supported performance verifications and to provide objective performance data to purchasers,
consulting engineers, and permitters of environmental technologies.

The MART Corporation (MART) has manufactured power washer cleaning equipment, designed
for use with aqueous alkaline cleaners, for over 26 years. Power washers generate a large
quantity of spent solution that is either evaporated or hauled away for treatment and disposal. In
response to this issue, MART developed the MART EQ-1™ System, which is a batch treatment
process that separates water from a waste stream in one step. The MART EQ-1™ System
consists of the EQ-1™ unit and an optional Final Polishing System (FPS). The MART EQ-1™
unit employs a proprietary chemical called "Magic Dust" to perform the separation of
contaminants such as oil/grease (O&G) and metals from the cleaning solution. The MART
process utilizes adsorption and electrostatic forces to encapsulate waste products including paint,
solid and dissolved metals (e.g., lead, cadmium, chromium), dust, oil, minerals, and even
asbestos. The encapsulated material (processed waste) cures and sets up like hardened dough or
concrete. The treated water and unused chemical are recycled.

Testing of the MART EQ-1™ system will be conducted at the 179th AW located in Mansfield,
Ohio. The 179th AW is charged with a mission of maintaining combat readiness and mobility to
deploy globally in the event of a national security action. The 179th AW is an Ohio ANG unit
that has Federal, state, and community roles. Its Federal role is to support the Unites States
Mlitary Objectives, through participation in America's Armed Forces. Its state role is to support
the Governor by providing trained units and equipment capable of protecting life and property,
and preserving peace, order, and public safety. Its community role is to be an active participant
in domestic concerns through local, state, and national programs. The major activities performed
at the Mansfield ANG include aircraft maintenance, aerospace ground equipment maintenance,
ground vehicle maintenance and facilities maintenance. The 179th AW has operations, logistics,
support, and medical professionals who provide airlift capabilities to serve the state and the
nation.

This project will evaluate the ability of the MART EQ-1™ Wastewater Processing System to
separate oil/grease, metals, and suspended solids from the spent cleaning solution. Evaluating
and verifying the performance of MART'S 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 to determine the efficiency of oil/grease, metals, and suspended solids
removal for a given set of operating conditions.

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The test plan described in this document has been structured based on a format developed for
ETV-MF projects. This document describes the intended approach and explains testing plans
with respect to areas such as test methodology, procedures, parameters, and instrumentation.
Also included in this test plan is Quality Assurance/Quality Control requirements of this task that
will ensure the accuracy of data, data interpretation procedures, and worker health and safety
considerations.

The test plan will be maintained at the test site, and verification testing will be conducted in strict
adherence to the test plan requirements. Any modifications to or deviations from the test plan
will be documented according to the procedures outlined in this test plan.

1.1 Background

The Federal electroplating and metal finishing pretreatment wastewater standards were
developed by EPA by identifying commonly used treatment practices and determining
their effectiveness by collecting effluent data from well operated systems. EPA selected
conventional wastewater treatment as the standard system. Therefore, for most plating
shops, the use of conventional treatment will provide sufficient pollutant removal to meet
discharge standards. Some conventional methods used for removal of metals from
wastewater include: (1) hydroxide precipitation techniques; and (2) sludge de-watering
using gravity thickening followed by a mechanical de-watering device to increase the
solids content of the sludge and therefore reduce its volume.

There are two major exceptions to this rule. First, many plating shops are regulated by
local discharge standards that are more stringent than the Federal standards, and
conventional treatment may be insufficient to meet these limitations. Second, the
treatment system selected by EPA for establishing Federal standards were those systems
that EPA determined to be "properly operating facilities." For example, EPA omitted
facilities that: (1) did not have well operated treatment processes; (2) had complexing
agents (e.g., non-segregated wastes from electroless plating); and (3) had dilution from
non-plating wastewaters. Consequently, some plating facilities may not meet the properly
operated facility criteria used by EPA and may have difficulty meeting Federal and/or
local discharge standards using conventional treatment. In light of many facilities that
may have difficulty cost-effectively meeting applicable discharge standards using
conventional methods, there is a need for innovative wastewater treatment technologies.
A cost-effective, waste minimization process that can effectively treat wastewater will
have the desirable effects of water reuse, reduction in generation of hazardous waste,
reduction in hazardous waste disposal costs, reduction in raw material costs, and
ultimately, regulatory compliance when discharging.

2.0 TECHNOLOGY DESCRIPTION

2.1 Theory of Operation

The MART EQ-1™ Wastewater Processing System (Figure 1) is an inventive
technology that chemically separates and clarifies the wash solution and encapsulates the

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waste for disposal. The MART process utilizes adsorption and electrostatic forces to
encapsulate waste products. The chemical compound used in the MART encapsulating
process is a non-hazardous proprietary product called Magic Dust, which is formulated
for the specific site and application.

The heart of the MART EQ-1™ process is based on the performance of the Magic Dust.
The Magic Dust is a blend of clay, polymeric, acidic, and various other additives that
allow the compound to integrate several reactions in one. The function of the Magic Dust
is as follows: (1) The acidic components cause oily contaminants to coalesce and separate
from the wastewater; (2) the polymeric cationic portion attracts any remaining oils and
the larger, more highly charged anions; (3) the third component group precipitates
metallic hydroxides and drives the system to a fully flocculated condition where the clay
particles attract the cationic polymer molecules (with absorbed oil), metallic ions and
positively charged contaminants; and (4) the heavy metal cations still remaining in
solution exchange with sodium in the clay and electrostatically bond to the clay platelets.
The fully reacted mass is a complex mixture of encapsulated contaminants and waste
solids that are held together by van der Waals as well as electrostatic forces. The clay
particles agglomerate, completely entrapping and surrounding suspended solids.
Pozzolanic reactions also occur, which form cement-like particles that settle to the
bottom of the reaction vessel.

Figure 1: The MART EQ-1™ Unit

The Magic Dust is added to the wastewater and the agglomerate is mixed to cause the
necessary complex reactions and microencapsulation: molecules with adsorbed oil,
metallic ions, and charged contaminants are attracted to the Magic Dust to form a mass.
The Magic Dust formulation also includes chemistry to demineralize the treated water
After microencapsulation, the flocculated waste is filtered through a disposable media
paper to collect the waste for disposal. The encapsulated waste is collected in the filter
paper and the clarified solution is collected in a holding tank. The filter paper containing
the encapsulated waste is rolled up and allowed to harden into a cement-like material.
The filter paper and waste material are put into a drum and disposed of off-site as

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hazardous waste. The clarified solution can be recycled and reused or treated further with
an optional FPS and discharged to the sanitary sewer. The MART FPS is a basic ion
exchange system that utilizes a granular activated carbon filter along with a polymer resin
chamber, which employs polystyrene beads with sodium ions as the resin media. The
pre-filter removes oil/grease, and other contaminants that may hinder the effectiveness of
the beads. Next, the solution is sent through the resin chamber where heavy metals are
removed.

2.2	Commercial Status

The MART EQ-1™ Technology was introduced into the market in January 1998. Since
the product launch, the Navy, Air Force, and Marines have utilized the EQ-1™, as have
industrial companies wanting to reduce waste and disposal costs. MART currently has
64 units installed.

2.3	Pollution Prevention Classification

The MART EQ-1™ is a wastewater recycling technology. MART has manufactured
Power Washer cleaning equipment for over 26 years. The Power Washer is designed for
use with aqueous alkaline cleaners. Many of MART's customers over the years have
relied on the expensive services of waste haulers to remove and transport the spent
solution from the Power washer. In response to MART's customers' need for solution
maintenance, they launched the MART EQ-1™ in January 1998. The EQ-1™ focuses on
the recycling of water used in cleaning processes.

2.4	Environmental Significance

The MART EQ-1™ is employed to: (1) reduce the quantity of fresh water needed in the
cleaning process, by recycling treated water back into the original process, (2) reduce the
volume of sludge and teachability of heavy metals in the hazardous sludge, and (3)
remove heavy metals, and oil/grease from the discharged waste stream.

3.0 PROCESS DESCRIPTION

3.1 Equipment and Flow Diagram

The MART EQ-1™ unit is equipped with two connecting tanks (Figure 2): a
mixing/reaction tank (upper reservoir tank) and a holding tank (lower reservoir tank).
Each tank is made of sheet steel and has a capacity of 125 gallons. The upper tank is of a
trapezoidal design; this is where the untreated water is pumped and the treatment
chemical (Magic Dust) is added. Once the solution is thoroughly mixed the encapsulated
material is allowed to settle to the bottom of the mixing/reaction tank. A sight glass is
provided on this tank so that the separation/encapsulation process can be observed.

After encapsulation the treated water is allowed to drain into the holding tank. The
treated water flow is controlled by two separate ball valves located at the bottom of the

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upper tank. Both valves are two inches in diameter and are operated manually. The
standpipe valve controls the flow of the clarified solution and light flocculation, and the
bottom valve controls the flow of heavy precipitation. The standpipe, located on the
inside of the upper tank, can be cut to adjust the height of the pipe to the depth of the
flocculated material.

All treated water is allowed to pass through a filtration media (30 micron (|i) paper)
before entering the holding tank. The MART system contains a metal filter pan, directly
below the upper tank, to hold the filter media. The filter media is constructed of rayon
fiber and collects the treatment chemical with the encapsulated waste. As the waste is
collected on the filter paper, the paper is slowly pulled forward and wrapped around the
encapsulated waste. When the waste has been sufficiently wrapped, the filter paper is cut.
The encapsulated waste is removed and placed in the drying tray, which is located on the
right side of the unit. This process is repeated until all the wastewater has been processed.
As the encapsulated waste is rolled in the filter paper, the paper is squeezed to remove
excess solution. The clarified solution in the holding tank is transferred with a
submersible pump to the FPS, which is an optional secondary treatment.

The FPS is a basic ion exchange system. The system is cationic and polystyrene beads
with sodium ions are used for the resin media. The FPS includes a granular activated
carbon filter along with a polymer resin chamber. The clarified solution enters the pre-
filter carbon media to remove oil, grease, and other contaminants. The filtered solution
then enters the ion exchange chamber, where the metal ions are removed by being
captured on the beads. The pre-filter chamber is 3" in diameter, 25" tall, and requires one
20" -15 |i filter cartridge. The refillable resin chamber has a polyvinyl chloride (PVC)
shell with a 250 |i polypropylene strainer. The strainer prevents resin migration with the
solution. The resin has a 1 pound (lb.) per 0.5 cubic feet (ft3) capacity. The specification
for the FPS is 72 gallons per hour (gph) or 1-2 gallons per minute (gpm) for maximum
removal efficiency.

3.2 Testing Site

The test site selected for verification of the MART EQ-1™ system is the Ohio ANG
179th AW in Mansfield, Ohio. The 179th AW has a 52 year history from the early days
organizing the 179th unit and flying fighters, to their present day situation as a first string
member of the Total Force and flying the C-130 Hercules (C-130H) aircraft. The 179th is
an Air Force ANG comprised of 950 personnel, with about 250 being full-time. Their
primary mission is to provide airlift capabilities for the state of Ohio and the U.S.

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Figure 2: The MART EQ-1™ Schematic	Legend:

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The 179th AW utilizes the C-130H transport in their daily airlift capabilities
operations. The 179th AW cleans the engines on their eight C-130H aircraft at least
once each year as preventative maintenance to ensure maximum performance, as well
as aircraft and aircrew safety. In 1993, cadmium was detected in the engine
compressor spent wash wastewater. The cadmium rinsate was believed to be coming
from the cadmium-plated internal compressor blades in the C-130H aircraft engine.
At that time most of the Department of Defense (DOD) facilities were not collecting
their spent wash wastewater. Consequently, in 1994 the ANG Headquarters (HQ)
stated that there was a possible problem and in 1995 instructed all C-130H bases to
stop aircraft engine washing until a collection system could be developed. In 1997
engine compressor washing resumed. The spent wash wastewater was collected and
drummed as hazardous waste, using a wastewater collection container.

The spent wash wastewater collected from the cleaning of the C-130H engines has
the potential to generate large quantities of hazardous waste annually at each ANG
base. The 179th AW realized this environmental impact and began implementing a
program to treat the C-130H engine compressor spent wash wastewater at their site,
as well as their spent aqueous- based parts washer water.

3.3 The 179th AW C-130H Engine Cleaning Process

It is a requirement at the 179th AW to wash the C-130H aircraft engines at least once
each year to ensure maximum performance and aircraft and aircrew safety. The
cleaning process used at the 179th AW is as follows:

•	Soap application (soak for 5 minutes)

•	Soap application again (soak for 20 minutes)

•	2 clean water rinses

The aircraft cleaning solution used is Eldorado ED-563. The Material Data Safety
Sheet (MSDS) is provided in Appendix A. The entire cleaning process generates no
more than 10 gallons of water/soap rinsate per engine and no more than 40 gallons
per plane. This results in the generation of approximately 640 gallons of wastewater
per year at the 179th AW base. The rinsate mixture is comprised of approximately
94% water, 5% soap, and 1% cadmium and oil/grease. Table 1 presents background
analysis of a C-130H engine spent wash wastewater sample taken before treatment. It
was collected by the 179th AW on October 20, 1997 and tested by Clayton Laboratory
Services. The spent wash wastewater is hazardous for cadmium at 11 ppm. The
cadmium in the rinsate comes from the cadmium-plated internal compressor blades of
the engine. The oil/grease in the rinsate come from the engine. It is a mixture of oils
and carbon from the exhaust. It is estimated that the concentration of contaminants in
this spent wash wastewater remains relatively constant, because the frequency of C-
130H engine cleanings is determined based on the number of hours the engine is in
service.

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Table 1. Spent Engine Cleaning Wash Wastewater Background Analysis

Constituent

Unit

Parameter

Cadmium (Cd)

PPm

11

Oil/Grease

PPm

2500

pH

pH units

7.1

After the four C-130H aircraft engines on each plane are cleaned, the cleaning
solution and rinsate are collected in a large 500 gallon plastic polystyrene collection
container (Figure 3) and transported to the MART system. The treated engine wash
wastewater is discharged to the POTW.

Figure 3: The 179th AW Wash Wastewater Collection Container

3.4 The 179th AW Parts Washer Cleaning Process

There are three part washers at the 1791'1 AW, each of which utilizes an aqueous based
alkaline cleaner. MSDSs for each of the cleaner's are provided in Appendix A. A
description summary of the washers is presented in Table 2 The alkaline cleaners are
treated individually, by the MART unit. The spent alkaline cleaners contain soils
which are primarily cadmium (Cd), chromium (Cr), paint chips, and oil/grease. Some
of the minor contaminants include lead (Pb), barium (Ba), nickel (Ni), and copper
(Cu). The spent alkaline cleaner concentration varies depending on the type and
quantity of soil on the parts and age of the cleaning solution. After treatment in the

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MART system the treated alkaline cleaner is pumped back into a tank and than to be
used in the parts washer area.

Table 2. Parts Washers at the 179th AW

Parts Washer

Size
(Liters)

Alkaline
Cleaner

Use

Contaminants

Engine Shop
(MARTฎ Tornado
40)

680

DARACLEANฎ
235

Aircraft
engine
panels

Cd, Cr, Cu, Pb,
Oil/grease

Aircraft Ground
Equipment (AGE)
(MARTฎ Cyclone 30)

490

DARACLEANฎ
282

Burner cans
from engine
heater

Cd, Cr, Pb, Ba,
Oil/grease

R&R (Tire Shop)

(MARTฎ Cyclone 30)

490

DARACLEANฎ
282

Rims, bolts,
& various

brake
components

Cd, Cr, Cu, Ni,
Ba, Oil/grease

4.0 EXPERIMENTAL DESIGN

4.1 Test Goals and Objectives

The overall goal of this ETV-MF project is to evaluate the ability of the MART EQ-
1™ system to separate oil/grease, metals, and suspended solids from the spent
cleaning solution. This technology will be evaluated under actual production
conditions, and the operation of the unit will be characterized through the
measurement of various process control factors.

The following is a summary of specific project objectives. Under normal system
operating set-points at the 179th AW and varying contaminant-loading rates:

•	Prepare a material balance for wastewater constituents (soils and metals)
in order to:

1)	Evaluate the ability of the MART EQ-1™ system to remove
oil/grease and metals.

2)	Evaluate the ability of the MART EQ-1™ system to recycle
cleaner solution.

•	Determine the cost of operating the wastewater processing system for
the specific conditions encountered during testing.

1) Determine labor requirements needed to operate and maintain the
MART EQ-1™ system.

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2) Determine the quantity of energy consumed by the MART EQ-1™
system during operation.

•	Quantify the environmental benefit by determining the potential for

reduction in water and chemical disposal frequency.

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.

The following are critical measurements:

•	Magic Dust chemical additions (lbs.) and related costs

•	Treated waste volumes (L) and related costs

•	Total Suspended Solids (TSS) of system influent and effluent streams

•	Cleaner concentration (system influent and effluent streams for EQ-1™
and FPS based on alkalinity and refractive index or conductivity)

•	Conductivity of the influent and effluent streams

•	Oil/grease concentration (system influent and effluent streams for EQ-
1™ and FPS, encapsulated waste)

•	Metal concentration (system influent and effluent streams for EQ-1™
and FPS, and encapsulated waste)

•	Operation and Maintenance (O&M) labor requirements (hours) and
costs

•	Energy use (kilowatt-hour (kWh)) and costs

•	Quantity and chemistry of the encapsulated hazardous solids

•	Air monitoring (cadmium and chromium)

The following are non-critical measurements:

•	pH of the influent

•	Flocculation formation time

•	Settling time

4.3	Test Matrix

Testing will be conducted in four distinct test periods, with each test period having a
batch (60 - 100 gallons) processed through the MART EQ-1™ system. The
conditions for each test are outlined in the sections below. Test objectives and
measurements are summarized in Table 3.

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Table 3. Test Objectives and Related Test Measurements for Evaluation of the MART EQ-1™ System

Test

Test Objective

Test Measurement

1. Typical

contaminant loading
rate found in the C-
13 OH engine
wastewater.

Prepare a material balance for wastewater constituents (soils
and metals).

•	Chemical characteristics of feed solution.

•	Chemical characteristics of recovered product.

•	Volume and chemical characteristics of wastes removed from
wastewater.

•	Quantity of fresh cleaning chemicals added during testing.

Evaluate the ability of the MART system to process spent
cleaner solution and separate usable cleaner solution
chemistry from contaminants.

•	Chemical characteristics of feed solution.

•	Chemical characteristics of recovered product.

Determine the cleaner recovery rate of the system,
normalized based on production throughput and soil loading.

•	Volume of product produced.

•	Production throughput for wastewater.

•	Soil loading.

Determine labor requirements needed to operate and
maintain the MART system.

• O&M labor required during test period.

Determine the quantity of energy consumed by the MART
system during operation.

• Quantity of energy used by pumps and mixer.

Determine the cost of operating the wastewater recycle
system for the specific conditions encountered during
testing.

•	Costs of O&M labor, materials, and energy required during test
period.

•	Quantity and price of fresh cleaning chemicals added during testing.

Determine if worker exposure is elevated, as a result of
operating the MART system.

• Perform air monitoring at a low and high soil load level.

Quantify/identify the environmental benefit.

• Review historical waste disposal records and compare to current
practices.

2. High contaminant
loading rate using
the R&R parts
washer wastewater.

Same as above.

Same as above.

3. High contaminant
loading rate using
the AGE parts
washer wastewater.

Same as above, with the exception of worker exposure
analysis.

Same as above, with the exception of air monitoring.

4. High contaminant
loading rate using
the Engine Shop
parts washer
wastewater.

Same as above, with the exception of worker exposure
analysis.

Same as above, with the exception of air monitoring.

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4.3.1	Engine Spent Cleaning Wash Wastewater - Test #1

During the first test period, the MART EQ-1™ system will be operated using
normal operating conditions found at the 179th AW (Section 3.3). A "typical"
level of contamination found when treating spent engine wash wastewater will be
used during this test period. This "typical" level can be defined as the normal
contamination load in the wastewater after being used to clean the C-130H
engine. This "typical" level will be quantitatively determined during the first test
period by collecting and analyzing representative samples of the feed solution.

4.3.2	Parts Washers' Wastewater - Test #2-4

During the second through fourth test periods, the MART EQ-1™ system will be
operated using normal operating conditions found at the 179th AW (Section 3.4).
Test #2 will evaluate the ability of the MART EQ-1™ to remove contaminants in
the R&R parts washer wastewater, Test #3 evaluates the AGE parts washer
wastewater, and Test #4 the Engine Shop parts washer wastewater. The
wastewater from the parts washers has historically contained a higher
concentration of heavy metals, specifically cadmium, than the engine wastewater.
To evaluate the operation of the MART EQ-1™ system under a higher
contamination loading condition, the parts washers' wastewater will be processed
through the MART™ unit. The higher contaminant loading level will be
quantitatively determined for each of the parts washer streams during the
respective test period by collecting and analyzing samples of the feed solution.

Testing and Operating Procedures

4.4.1 Set-Up and System Initialization Procedures

Prior to startup, the MART unit will be flushed with fresh water. The procedure is
as follows:

•	Position the filter paper to fully cover the metal filter pan.

•	Close discharge line valve.

•	Fill mixing/reaction tank with fresh water. Rinse walls of tank.

•	Open the bottom valve and standpipe valve.

•	Allow water to drain through both valves, into the Holding tank, until the
mixing/reaction tank is empty.

•	Start the holding tank transfer pump.

•	Pump rinse water through transfer pump, until adequately cleaned.

•	Drain holding tank.

•	Close bottom valve, standpipe valve and other discharge valves on MART
unit.

•	Remove filter paper and appropriately dispose of it.

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The mixing/reaction tank will then be filled with 60 to 100 gallons of wastewater
solution and the MART EQ-1™ unit will be started according to instructions in
the O&M manual (Appendix B).

4.4.2 System Operation

The unit will be operated on a batch basis, with 60 - 100 gallons processed during
each test cycle. Only one batch will be sampled per test cycle. At the completion
of the first test cycle, the unit will be drained and cleaned and restarted following
the same procedures as those used for set-up and system initialization.

The operation of the MART system will be as follows:

•	Mx the wastewater in the collection container for 5 minutes to
assure that the wastewater soils and oil/grease have not separated
and verify that the pH is above 7.0 using pH paper.

•	Transfer 60 - 100 gallons of wastewater from the collection
container into the upper reservoir of the MART system, using a
pump and commercial duty hose.

•	Turn on reservoir mixer to mix wastewater 45 - 60 seconds.

•	Add Magic Dust to wastewater.

•	Within the upper reservoir the wastewater is mixed with the Magic
Dust at the ratio outlined in Table 4. A portable electronic scale will
be used to accurately measure the Magic Dust quantity. A
calibration mass will be utilized for calibration of the electronic
scale.

Table 4: Magic Dust Addition to Wastewater

Wastewater Stream

Formulation
Number

lbs. Magic Dust per
100 gal. Wastewater1

C-130H Engine
Wastewater

29498-73105

6.0 - 8.0

Engine Shop Parts
Washer

29498-73105

6.0 - 8.0

AGE Parts Washer

29498-73104

6.0-8.0

R&R Parts Washer

29498-73105

6.0 - 8.0

•	Allow to mix for 5 minutes.

•	Shut off mixer and observe formation of flocculent in sight glass for
5 minutes. If no flocculent is observed, add 0.5 lbs. Of Magic Dust.
Allow to mix for 5 minutes. Shut off mixer and observe flocculent.

1. The additions of Magic Dust are for typical soil loading and may vary with light or heavy soil loading.

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Continue in this manner, with 0.5 lbs. Magic Dust increments, until
flocculent is observed.

•	Prepare filter paper for discharge of clarified solution and
encapsulated waste. Roll paper out to cover the filter pan above the
holding tank.

•	Once separation between the encapsulated waste (flocculent) and
clarified solution occurs, open the standpipe valve.

•	Discharge clarified solution through the filter paper and into the
holding tank.

•	Close standpipes valve and open bottom valve.

•	Discharge encapsulated waste onto filter paper.

•	When a significant quantity accumulates on the filter, close the
bottom valve and wrap the filter paper around the encapsulated
waste.

•	Squeeze out clarified solution when wrapping waste in the filter
paper.

4.4.3 Sampling and Process Measurements

4.4.3.1 Sampling Responsibilities & Procedures

Sampling and process measurements for the R&R parts cleaner and engine

parts cleaner will be taken according to the schedule presented in Table 5.

Sampling events and process measurements will be recorded on the form

shown in Figure 4.

Sample ports will be installed to collect feed and product samples from the

MART unit (see Figure 2 for sample locations).

Table 5. Sampling Frequency and Parameters to Be Measured

Sample
Name

Sample
Location

Frequency/
Type

Parameters

Wastewater
Influent

Wastewater In

MARTEQ-

l™unit

2 grab

samples/batch

O&G, TSS, Alkalinity, Cd, Cr,
Pb, Ba, Ni, Cu , Conductivity,
Refractive Index

Wastewater
Effluent/FPS
Influent

Wastewater
Out MART
EQ-1™ unit

2 grab

samples/batch

O&G, TSS, Alkalinity, Cd, Cr,
Pb, Ba, Ni, Cu, Conductivity,
Refractive Index

Encapsulated
Waste

Filter Pan

2 grab

samples/batch

O&G, Cd, Cr, Pb, Ba, Ni, Cu,
TCLP Metal

* Refractive Index will be measured when Daraclean 235 is used. Conductivity will be measured
when Daraclean 282 is used.

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Figure 4. Data Collection Form

Test # :	 Date:	Batch # :		Operation: MART EO-1™ System

Revision #: 0	Revision Date: Original	Technology Type: Water Recycling

Date/
Time

Initials

Sample
Number

Sample
Location

MART EQ-1™
Influent Stream

MART EQ-1™
Effluent /FPS
Influent Stream

MART FPS Effluent
Stream

Settling

Time
(minutes)

Flocculation
Time
(minutes)

Notes and Observations

Conductivity/
Refractive Index

(% Bx)

Conductivity/
Refractive Index

(% Bx)

Conductivity/
Refractive Index

(% Bx)





























































































































































































































Total Wastewater Flow into MART EQ-1™ (L)	

Total Wastewater Flow out of MART™ FPS (L)	

Page	of

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For the engine wash water and AGE parts washer, three samples for all
parameters plus two extra O&G (total of five) will be collected. In
addition, three samples for all parameters plus two extra O&G (total of
five) will be collected from the FPS during the wash wastewater test.
These samples are field duplicates and for laboratory QA/QC analyses
identified in Sections 5.2.2.1 and 5.2.2.2.

The appropriate sampling container will be used for each test parameter,
as outlined in this Test Plan. Each laboratory sample bottle will be labeled
with the date, time, sample identification, and test parameters required.

Samples to be analyzed at off-site laboratories will be accompanied by a
chain of custody form. The samples will be stored and transported in
appropriate sample transport containers (e.g., coolers with packing and ice
packs or bags of ice) by common carrier. Security sealing tape will be
applied to the transport containers to ensure sample integrity during
delivery process to the analytical laboratories. A Project Team Member
will perform sampling and labeling, and ensure that samples are properly
stored and secured for transport to the analytical laboratories. Each
sample will be taken in duplicate with the duplicates to be shipped in a
separate shipping container.

4.4.3.2 Process Measurements

The conductivity of the influent and effluent streams will be measured
using digital analyzers. The refractive index will be measured with a
refractometer. Calibration of the process measurement equipment will be
performed daily, according to suggested manufacturer recommendations.

Electricity use will be calculated by determining the power requirements
and cycle times of pumps and other powered devices. The 179th AW will
provide the cost of labor, electricity, and other items needed for a cost
analysis.

Process fluid flowrates for this demonstration will be measured by Omega
Engineering, Inc., Model FD-7000 liquid flowmeter. It is a multi-liquid
ultrasonic flowmeter with non-penetrating transducers.

4.4.3.2.1 Calibration Procedures and Frequency

The following procedures will be used to calibrate the
instruments/equipment that will be used to collect process
measurements:

1. Instruments used to perform analytical methods will be
calibrated according to the laboratory quality assurance plan.

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2.	Instalments used to conduct air sampling and analysis will be
calibrated according to equipment manufacturer's
specifications and Safety Compliance's and DLZ Laboratories,
Inc. specific quality assurance plan's.

3.	The ultrasonic liquid flowmeter will be calibrated at the start of
each sampling day, in accordance with the equipment
manufacturer's instructions.

4.	The conductivity meter and refractometer will be calibrated at
the start of each sampling day, and in accordance with the
equipment manufacturer's instructions. Manufacturer, nominal
value, lot number and expiration date of standard solutions
used will be recorded on the data collection form and project
notebook.

The on-site Project Team will perform field measurements, as
well as calibration of field equipment.

4.5 Test Parameters

A summary of the sample analysis and handling requirements to be used during the
verification test is presented in Table 6. Details of the test parameters to be performed are
outlined in the ensuing sections.

4.5.1	Oil/Grease Concentration

The MART EQ-1™ system will be verified to determine its effectiveness at
removing oil/grease from the spent cleaning wastewater. A gravimetric method
for measuring organic soils in aqueous and sludge samples was selected for
analytical testing. The selected samples will be acidified with 50% hydrochloride
acid to lower the pH to less than 2. The method chosen was Standard Methods
for the Examination of Water and Wastewater 20th Edition 1998 (SM) 5520B
(20th edition), which uses n-hexane as the extraction solvent. The method is a
liquid/liquid extraction, gravimetric procedure applicable to aqueous matrices for
the determination of n-hexane extractable materials. Obtaining the concentration
of oil/grease before and after the MART EQ-1™ and FPS will determine its
ability to remove oil/grease from cleaning wastewater. Oil/grease will be
extracted from the solids using SM 5520E prior to analysis by SM 5520B.

4.5.2	Cleaner Concentration

The MART EQ-1™ system will be verified to determine its effectiveness at
recovering cleaner from the wastewater. Obtaining the concentration of cleaner
before and after the MART EQ-1™ and FPS will determine its ability to recover
cleaner from wastewater.

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Table 6. Summary of Analysis and Handling Requirements

Parameter

Test Method

Sample
Bottle

Sample
Volume
Required

Preservation
/Handling

Hold
Time

Oil/Grease
Wastewater

SM Method
5520B

Glass jar

1000 ml

Acidify to
pH
<2
w/HCL

28 days











Oil/Grease
Solids

SM 5520E/
5520B

Glass jar

500 g

4ฐC

28 days

Total
Alkalinity

EPA Method
310.1

Glass jar

500 ml

4ฐC

Analyze
as soon
as

practical











TSS

EPA Method
160.2

Polyethylene

500 ml

4ฐC

7 days

Metals
Wastewater

EPA Method
200.7

Polyethylene

500 ml

Acidify to
pH < 2
w/HN03

6 months

Metals
Solids

SW-846
3050B/6010B

Polyethylene

500 g

4ฐC

.6 months

TCLP
Metals

SW 846
Method
1311/301 OA/
6010B

Polyethylene

500 g

4ฐC sample/
HN03 To
extract

6 months

A split sample from the solid waste samples will be dried at 100ฐC to constant weight to
determine percent moisture.

4.5.3 Metals

The wastewater at the 179th AW contains a large concentration of cadmium and
minute concentrations of other metals. The MART EQ-1™ and FPS will be
evaluated on its ability to effectively remove cadmium from wastewater. The test
will determine the cadmium concentration, as well as chromium, lead, barium,
nickel and copper in the wastewater influent and effluent and encapsulated waste
streams. The selected samples will be acidified with nitric acid to lower the pH to
less than 2. The method selected is the Inductively Coupled Plasma - Atomic
Emission Spectrometry, EPA Methods and Guidance for Analysis of Water
(EPA) Method 200.7 for aqueous samples. For the analysis of the solid waste
samples, the solid waste will be digested using EPA Test Methods for Evaluating
Solid Waste (SW-846) method 3050B prior to the analysis using method SW-846
Method 6010B. For Toxicity Characteristic Leaching Procedure (TCLP), SW-
846 Method 1311 will be used to leach solid waste samples, followed by digestion
using 3010A and analysis by 601 OB.

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4.5.4 Total Suspended Solids

To determine the effectiveness of the MART EQ-1™ and FPS unit with regard to
removal of particulates, tests for total filterable residue (EPA Method 160.2) will
be performed. The referenced method produces values commonly referred to as
total suspended solids (TSS).

4.6 Air Monitoring

Cadmium, lead, and chromates are currently used for corrosion control and	protection

against wear in coatings, sealants, and surface treatments. Using cadmium,	lead, and
chromates for these purposes is pervasive throughout the aerospace industry, both within

the Department of Defense and the commercial aircraft industry. Cadmium,	lead, and

chromium particles in air are a serious concern to health and safety	personnel.
Increasingly, workplace safety procedures include monitoring of toxic substances.

The goal of the ETV-MF Program is to verily the environmental performance
characteristics of commercial-ready technology through the evaluation of objective and
quality-assured data, an important component of this is to demonstrate that this emerging
technology does not increase worker exposure to toxic substances due to its operation.
To determine if there is a potential for exposure to cadmium (Chemical Abstract Number
(CAS#): 7440-43-9) and chromium (CAS#: 22541-79-3), air monitoring will be
conducted during operation of the MART unit and handling of encapsulated waste.
Testing will consist of monitoring during two separate tests. The tests include treatment
of the C-130H engine compressor wash wastewater and treatment of the R&R parts
washer wastewater.

Exposure air monitoring, on an employee who is suspected to be at the highest risk of
exposure, will occur during processing of two separate wastewater streams fed into the
MART unit. Samples of each of the wastewater streams will be taken prior to testing, in
order to determine the contaminant load level. Air monitoring will be conducted in
accordance with the National Institute of Occupational Safety and Health (NIOSH)
Method 7300. A 0.8 micron (pore size) cellulose ester, 37 millimeter (mm) diameter
filter will be used as the collection media. SKC personal air sampling pumps will be
utilized and calibrated before and after each sample to a rate of 1 liter per minute (Lpm).
The personal pumps will be used to draw the air onto the collection media. Calibration
will be performed utilizing a primary standard (MiniBuck) with a representative sample
in line. Two sets of sampling will be conducted during the same operation. One sample
for low-level exposure, and the other to determine the high-level exposure. A minimum
of two field blanks will be included in each sampling set and the total sampling time will
be approximately 7 hours. One 15-minute Short-Term Exposure Limit (STEL) sample
will be collected during the sampling period. Two Time Weight Average samples for a
period of 3.5 to 4.0 hours will also be collected. The samples will be sent to an American
Industrial Hygiene Association (AIHA)-accredited laboratory for analysis within 24
hours of collection. There will be a total of five samples per operation (STEL, time
weighted average (TWA) morning, TWA afternoon, and two field blanks). Unused

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collection media will be provided for blank matrix spike/blank matrix spike duplicate
determinations. A chain-of-custody form will accompany the samples to the laboratory.
Test data will be presented in a formal written report, which will include the laboratory
report and sampling sheets. The results will be appropriately compared with the OSHA 8-
hour TWA exposure limit.

5.0 QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS

Quality Assurance/Quality Control activities will be performed according to the applicable
section of the Environmental Technology Verification Program Metal Finishing Technologies
Quality Management Plan (ETV-MF QMP) [Ref. 1],

5.1	Quality Assurance Objectives

The first 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. The
second QA objective is to use standard test methods for laboratory analyses. The test methods to
be used are listed in Table 6.

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 identification (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. The form presented h Figure 4 will be used for recording data on-
site.

The on-site Project Team member will generate chain of custody forms, and these
forms will accompany samples when they are shipped off-site.

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 may be traced. The ETV-MF Program Manager will
maintain process-operating data for use in report preparation.

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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.

The Laboratory Manager shall be ultimately responsible for all final data released
from the laboratory. The Laboratory Manager or designee will review the final
results for adequacy to task QA objectives. If the manager or designee suspects
an anomaly or non-concurrence with expected or historical performance values,
or with task objectives for test specimen performance, 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 Laboratory Manager signs
and dates the final data package.

Data Reporting. The original report signed and dated by the Laboratory Manager
will be submitted to the ETV-MF Program Manager. A copy will be submitted to
the ETV-MF 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
SOP used for each parameter, the process or sampling point identification, the
final result and the units. The ETV-MF Program Manager shall retain the data
packages as required by the ETV-MF QMP [Ref. 1],

5.2.2 QA/QC Requirements

For those measurements where duplicates, spikes and spike duplicates are
inappropriate (e.g., flow totals, conductivity, and refractive index), duplicate
measurements will take place at the time of sampling. A minimum of three
repetitions will be conducted for each measurement (conductivity, and refractive
index) for each sampling day, in order to ensure compliance with the QA
Objectives stated in Table 7. The instrument will be calibrated if the objectives
for these measurements are not met.

5.2.2.1 Duplicates

Duplicate samples taken in the field will be used to quantify measurement

precision associated with the entire sampling and analysis system.

Duplicate analyses will be performed on influent, effluent, and solid waste

samples from the AGE parts washer and engine wash wastewater.

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5.2.2.2	Matrix Spikes

Matrix spike/matrix spike duplicates will be performed on influent,
effluent, and solid wastes from the AGE parts washer and the engine wash
wastewater. Sample splitting will occur in the analytical laboratory. For
air analysis, a blank matrix spike/blank matrix spike duplicate will be
performed for cadmium and chromium.

5.2.2.3	Field Blanks

A field blank will be taken at each sampling point at least for air analysis
once during the verification test period. Also, field blank sample of each
cleaner make up will be sent for analysis. This will ensure the ebsence of
matrix interference's for each sample matrix.

5.2.3 Calculation of Data Quality Indicators

Analytical performance requirements are expressed in terms of precision,
accuracy, representativeness, comparability, completeness, and sensitivity
(PARCCS). Summarized below are definitions and QA objectives for each
PARCCS parameter.

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Table 7: QA Objectives for Precision, Accuracy, And Detection Limits

Critical
Measurements

Matrix

Method

Reporting
Units

Method of
Determination

MDL

Precision
(RPD)

Accuracy
(% Recovery)

Completeness
(%)

O&G Concentration

Water

SM 5520B

mg/L

Gravimetric

5.0

+ 22

75 - 125

90



Solids

SM 5520E/
5520B

mg/L

Gravimetric

5.0

+ 22

75 - 125

90

Total Metals

Water

EPA 200.7

mg/L

ICP-AES

.001

ฑ25

75 - 125

95



Solids

SW-846
3050B/6010B

mg/L

ICP-AES

.001

ฑ25

75 - 125

95

TCLP Metals

Solid

SW-846 1311/
301OA/601OB

mg/L

ICP-AES

0.25

ฑ35

75 - 125

90

TSS

Water

EPA 160.2

mg/L

Gravimetric

1.0

ฑ 19.0

N/A

90

Total Alkalinity

Water

EPA 310.1

mg/L

Titration

1.0

ฑ10

85 - 115

95

Air Monitoring

Air

NIOSH 7300

(ig/m3

ICP

<2.0

<20

N/A

90

Flowrates:

















Wastewater Feed
(Influent)

Water

Flow Totalizer

liters (L)

-

-

< 10

N/A

90

Wastewater Product

fFffl i

Water

Flow Totalizer

liters (L)

-

-

< 10

N/A

90

(Effluent)

EPA: EPA Methods and Guidance for Analysis of Water	SW-846: EPA Test methods for Evaluating Solid Waste

SM: Standard Methods For the Examination of Water and Waste water 20th Edition 1998 NIOSH: NIOSH Manual of Analytical Methods

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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:

RPD = {(|Xi - X2|)/[(Xi + X2)/2]} x 100 =

RPD = relative percent difference

|x,-x2

(Xt +X2)
2

xlOO

where: Xi = larger of the two observed values
X2 = smaller of the two observed values

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 7.

For measurements, such as flowrate, where the absolute variation is more
appropriate, precision is usually reported as the absolute range, D, of
duplicate measurements:

D = | mi - m.2 I

where: D = absolute range

mi = first measurement
m2 = second measurement

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

x 100

where: P = percent recovery

SSR = spiked sample result

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SR = sample result (native)

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(s) that have been acquired for the MART system verification
testing. Analysis with spiked samples will be performed to determine
percent recoveries as a means of checking method accuracy. QA
objectives will be satisfied if the average recovery is within the goals
described in Table 7.

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 MART technology verification by the use of consistent
methods during sampling and analysis and by tractability of standards to a
reliable source.

5.2.3.4	Completeness

Completeness is defined as the percentage of neasurements 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 90 percent or greater as specified in Table 7.

5.2.3.5	Representativeness

Representativeness refers to the degree to which the data accurately and
precisely represent the conditions or characteristics of the parameter
represented by the data. For the purposes of this demonstration,
representativeness will be achieved by presenting identical analyte
samples to the specified lab(s) and executing consistent sample collection
and mixing procedures.

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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.

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 practical quantification limit
(PQL) will be laboratory qualified as "estimated."]

MDL is defined as follows for all measurements:

MDL = t(n-l,l-a = 0.99) X S

where: MDL	= method detection limit

t(n-u-a = o.99) = students t-value for a one-
sided 99% 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.]

5.2.4 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 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 difficult. The greatest
challenge is generally defining the system boundaries and what degree of
accuracy is required. Sampling, measurement, and analytical errors preclude

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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 5 illustrates the most fundamental form of the material balance equation.
Batch systems and continuous systems can both be modeled using this general
form.

Mass



Mass Input



Mass Output



Mass



Mass



Equals



Less

Plus



Less



Accumulation

Through



Through



Generated



Consumed

With the



System



System



Within the



Within the

System



Boundaries



Boundaries



System



System

Figure 5: Fundamental Material Balance Equation

Figure 6 illustrates the material flow into and out of MART system.

Cleaning Wastewater
Influent

Magic Dust

MART EQ-1™
Wastewater
Processing System

Treated Water
Effluent

Encapsulated Waste

Figure 6: Material Balance Equation For MART'S System

The goal of the MART verification project is to determine performance, which
can generally be measured in terms of efficiency. For solution maintenance
technologies, percent contaminant removal and percent solution recovery are
measures of system efficiency.

To determine efficiency, the fundamental material balance equation can be
simplified as:

Xi = Xs + Xe

where: Xi = Mass in influent
Xs = Mass in waste
Xe = Mass in effluent

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5.2.4.1	Cleaner Recovery Efficiency

Cleaner recovery efficiency can be determined by the following equation:

Crec (%) = [(Cprod x Prodvoi)/(Cfeed x Feedvoi)] X 100%

where: Crec	=	cleaner recovery efficiency

Cprod	=	product stream cleaner concentration (g/L)

Prodvoi	=	product volume collected during cycle (L)

Cfeed	=	feed solution cleaner concentration (g/L)

Feedvoi	=	feed solution volume processed during cycle (L)

5.2.4.2	Oil Removal Efficiency

Oil removal efficiency is determined by the following equation:

Oeff (%) = {[(0WX Wvoi) + (Oout x Prodvoi)]/(Oin x Feedvoi)} x 100%

where: Oeff	=	oil removal efficiency

Ow	=	oil concentration in waste stream (g/L)

Wvoi	=	waste stream volume processed during cycle (L)

Oout	=	product stream oil concentration (g/L)

Prodvoi	=	product volume collected during cycle (L)

Oin	=	feed solution oil concentration (g/L)

Feedvoi	=	feed solution volume processed during cycle (L)

5.2.4.3	Cadmium Removal Efficiency

Cadmium (Cd) removal efficiency is determined by the following

equation:

Cdeff (%) = {[(Cdwx Wvoi) + (Cdout x Prodvoi)]/Cdin x Feedvo)} x 100%.

where: Cdeff	=	Cd removal efficiency

Cdw	=	Cd concentration in waste stream (g/L)

Wvoi	=	waste stream volume processed during cycle (L)

Cdout	=	product stream Cd concentration (g/L)

Prodvoi	=	product volume collected during cycle (L)

Cdin	=	feed solution Cd concentration (g/L)

Feedvoi	=	feed solution volume processed during cycle (L)

5.2.5 Energy Use

Energy requirements for the MART unit will be calculated by summing the total
quantity of horsepower hours and dividing by 1.341 HP-hr/kWh to arrive at
electrical consumption.

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5.2.6	Cost Analysis

This analysis will quantify the accumulative cost benefit of the technology. The
costs for operating the MART unit at the 179th AW will be calculated to compare
operating costs for a time period prior to utilization of the unit. For the baseline
conditions, the most recent applicable data available, collected by the 179th AW,
will be used. The cost analysis will compare operating costs, including costs for:
chemical costs and savings, waste treatment/disposal cost and savings, labor,
utilities, maintenance and other materials.

5.2.7	Waste Generation Analysis

This analysis will quantify the environmental benefit of the technology. The waste
generation rates for operating the MART unit at the 179th AW will be calculated
and compared to waste generation rates for a time period prior to the installation
of the unit. For the baseline conditions, the most recent applicable data collected
by the 179th AW will be used. The waste generation analysis will consider
type/characteristics of waste generated, volume, and frequency of waste
generated.

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. 1] to ensure testing and data collection are performed according to the test
plan requirements. The decision to perform a quality audit, during this verification test, is
at the discretion of the ETV-MF Program Manager.

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.

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. 1],

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 analyses are
completed. Typically, these types of non-conformances are detected by the Laboratory

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Manager. In all cases of non-conformance, sample re-analysis will be considered as one
source of corrective action by the Laboratory Manager. 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 Task Leader 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 the
MART EQ-1™ system. The ETV-MF Program Manager, Donn Brown, will have
ultimate responsibility for all aspects of the technology evaluation. The ETV-MF Project
Manager assigned to this evaluation is Dr. A. Gus Eskamani. Dr. Eskamani and/or his
Project Team will be on-site throughout the test period and will conduct or oversee all
sampling and related measurements.

MART will be on-call during the test period for response in the event of equipment
problems. The 179th AW personnel will be responsible for operation of the MART EQ-
1™ equipment, related cleaning lines, and ancillary equipment such as pumps and system
instrumentation. The 179th AW personnel will also provide safety training as described in
Section 10 of this test plan. The ETV-MF Project Manager, and/or his Project Team, and
the 179th AW have the authority to stop work when unsafe or unacceptable quality
conditions arise.

AMTEST Laboratories, Inc., is responsible for analyzing verification test samples.
Director of Inorganic Laboratory Ms. Kathy Fugiel will be the point of contact.
AMTEST Laboratories is accredited for the analyses identified in this test plan.

Safety Compliance, Inc. is responsible for performing worker exposure air monitoring.
The Principal Scientist, Mr. Kelly Ruff, will be the point of contact. Safety Compliance,
Inc. will utilize an AIHA accredited laboratory, DLZ Laboratories, Inc., for the analyses
identified in this test plan.

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 (Appendix C), which will need to be submitted to the CTC
Program Manager for approval. Upon approval, the modification request will be assigned
a number, logged, and transmitted to the requestor for implementation.

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7.0 UTILITY REQUIREMENTS

The MART EQ-1™ and FPS are intricately wired together. The utility requirements include:

•	Electrical Service: 115 VAC, 60 Hz, single-phase

•	Submersible Transfer Pump: 30 gpm

•	Mixing Turbine: ]A hp, 1800 rpm

8.0 HEALTH AND SAFETY PLAN

This Health and Safety Plan provides guidelines for recognizing, evaluating, and controlling
health and physical hazards throughout the workplace. More specifically, the Plan specifies for
assigned personnel, the training, materials, and equipment necessary to protect themselves from
chemical hazards, and any waste generated by the process.

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. The 179th AW Hazard
Communication Program will be reviewed during training and will be reinforced
throughout the test period. All appropriate MSDS forms will be available for chemical
solutions used during testing.

8.2	Emergency Response Plan

The 179th AW has a contingency plan to p"otect 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 will be provided with appropriate personal protective
equipment (PPE) and any training needed for its proper use, considering their assigned
tasks. The use of PPE will be covered during training as indicated in Section 10.

The following PPE will be required and must be worn at all times when operating the
MART unit and when handling waste: neoprene gloves and safety glasses with side-
shields.

8.4	Lockout/Tagout Program

The facility lockout/tagout program will be used if necessary.

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8.5	Material Storage

Any materials used during the project will be kept in proper containers and labeled
according to the 179th AW requirements. Proper storage of the materials will be
maintained based on associated hazards. 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. Spill kits will be strategically located in the project
area. These kits contain various sizes and types of sorbents for emergency spill clean up.
Emergency spill clean up will be performed according to the 179th AW Emergency
Response Plan.

9.0 WASTE MANAGEMENT

The MART unit will be tested on processes already in place and operating at the 179th AW. This
equipment currently generates solid waste, as a result of being processed through the MART
unit. This waste material is presently collected and treated off-site, while the clarified solution is
discharged to the local Publicly Owned Treatment Works (POTW).

During testing, no additional wastes will be generated other than the normal treated quantities.
The 179th AW, using their normal practices, will handle this waste appropriately. Therefore, no
special or additional provisions for waste management will be necessary.

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. 2],

The purpose of this JTA Plan is to outline the overall procedures for identifying the hazards and
quality issues and training needs for each verification test project. This 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-MF Operation Planning Checklist
(Appendix D) will be used as a guideline for identifying potential hazards, and the Job Training
Analysis Form (Appendix E) 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 F). Health and safety training will be coordinated
with 1st Lt. Troy Cramer of the 179th AW.

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11.0 REFERENCES

1.	Concurrent Technologies Corporation, "Environmental Technology Verification
Program Metal Finishing Technologies (ETV-MF) Quality Management Plan,"
December 9, 1998.

2.	Concurrent Technologies Corporation, "Environmental Technology Verification
Program Metal Finishing Technologies (ETV-MF) Pollution Prevention
Technologies Pilot Job Training Analysis Plan," May 10, 1999.

12.0 DISTRIBUTION

Alva Daniels, EPA (3)

Jim Potthast, MART

IstLt. Troy Cramer, 179th AW, Ohio ANG

Gus Eskamani, CAMP, Inc. (2)

Donn Brown, CTC {3)

Clinton Twilley, CTC

Safety Compliance, Inc.

AMTest Laboratories

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APPENDIX A
179th AW Cleaner MSDSs

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APPENDIX B
The MART EQ-1™ System O&M Manual

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APPENDIX C
Test Plan Modification Request

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TEST PLAN MODIFICATION REQUEST

Date:	 Number:	 Project:	

Original Test Plan Requirement:	

Proposed Modification:	

Reason:

Impact:

Approvals:

Requestor:	

Project Manager:_
Program Manager:

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Test Plan Modification Requests

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 insure 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.
Program management 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 project manager. The
form should then be transmitted to the CTC program manager 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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APPENDIX D
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.

Project Name: 		Expected Start Date:

ETV-MF Project Manager: 			

Will the operation or activity involve the following:	Yes No Initials & Date

Completed

1. 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.







2. Equipment requiring special fire prevention precautions? (e.g. Class D
fire extinguishers)







3. Modifications to or impairment of building fire alarms, smoke

detectors, sprinklers or other fire protection or suppression systems?







4. Equipment lockout/tagout or potential for dangerous energy release?

Lockout/tagout requirements must be documented in Test Plan.







5. Working in or near confined spaces (e.g., tanks, floor pits) or in
cramped quarters?







6. Personal protection from heat, cold, chemical splashes, abrasions, etc.?

Use Personal Protective Equipment Program specified in Test Plan.







7. Airborne dusts, mists, vapors and/or fumes? Air monitoring,

respiratory protection, and /or medical surveillance may be needed.







8. Noise levels greater than 80 decibels? Noise surveys are required.
Hearing protection and associated medical surveillance may be
necessary.







9. X-rays or radiation sources? Notification to the state and exposure
monitoring may be necessary.







10. 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.







11. 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.







12. 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.

Project Name:

ETV-MF Project Manager:

Will the operation or activity involve the following:	Yes No Initials & Date

Completed

13. Processing or recycling of hazardous wastes? Special permitting may
be required.







14. Generation or handling of waste?







15. 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.







16. Contractors working in CTC facilities? Follow Hazard Communication
Program.







17. Potential discharge of wastewater pollutants?







18. EHS aspects/impacts and legal and other requirements identified?







19. Contaminants exhausted either to the environment or into buildings?

Special permitting or air pollution control devices may be necessary.







20. 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;	(Daiej

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APPENDIX E

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 F
ETV-MF Project Training Attendance Form

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ETV-MF Project Training Attendance Form

ETV-MF Project:

Date
Training
Completed

Employee Name

Last First

Training Topic

Test
Score
(If applic.)









































































































































































ETV-MF Project Manager:

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