Document ID: EPA-HQ-OPPT-2003-0012-0197
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2003-09-16T04:00Z

Mary
Dominiak
09/
15/
2003
08:
39
AM
To:
Mary
Dominiak/
DC/
USEPA/
US@
EPA
cc:
(
bcc:
Mary
Dominiak/
DC/
USEPA/
US)
Subject:
TRP
and
FMG
Materials
for
PFOA
ECA
Technical
Workgroups,
9/
16­
17/
2003
You
are
receiving
this
message
because
you
have
expressed
an
interest
in
receiving
information
concerning
the
Agency's
enforceable
consent
agreement
(
ECA)
process
on
perfluorooctanoic
acid
(
PFOA)
and
the
fluorinated
telomers,
OPPT­
2003­
0012.
If
you
no
longer
wish
to
receive
this
information,
please
reply
to
dominiak.
mary@
epa.
gov
requesting
that
you
be
removed
from
this
notification
list.

****************************************************************************************
TO:
PFOA
ECA
Technical
Workgroup
and
Plenary
Meeting
Attendees
Attached
are
materials
provided
by
the
Telomer
Research
Program
(
TRP)
and
the
Fluoropolymer
Manufacturers
Group
(
FMG)
for
use
and
discussion
at
the
PFOA
ECA
Technical
Workgroup
meetings
on
September
16
and
17,
2003.
The
attached
files
consist
of
the
draft
presentation
for
TRP's
degradation
study
proposal;
the
TRP
draft
telomer
incineration
test
protocol;
and
the
FMG
draft
fluoropolymer
incineration
test
protocol.
These
are
the
materials
which
TRP
and
FMG
committed
to
provide
during
the
Expert
Subgroup
meetings
conducted
on
August
14
and
19,
2003.
The
summaries
of
those
Subgroup
meetings
appear
in
the
docket
at
OPPT­
2003­
0012­
0195.

If
you
have
any
questions,
or
if
you
experience
any
difficulty
in
opening
the
attached
files,
please
contact
me.

Sincerely,

Mary
F.
Dominiak
U.
S.
Environmental
Protection
Agency
EPA
East,
Mail
Code
7405M
1200
Pennsylvania
Avenue,
NW
Washington,
DC
20460
Phone:
202­
564­
8104
Fax:
202­
564­
4775
Courier
deliveries:
1201
Constitution
Ave.,
NW,
Room
4410;
564­
4760
Test
Protocol
Outline
9­
12­
03­
FluoropolymeDRAFT
16­
Sept­
03
TRP
Detailed
Test
Protocol
Outli
DRAFT
16­
Sept­
03
TRP
Degradation
Presentatio
TRP
Telomer
Research
Program
Telomer
Technical
Work
Group
Meeting
Telomer­
based
Polymeric
Products
(
TBPP)
Biodegradation
Study
Strategy
16
September
2003
2003­
16­
09
,
page
2
Telomer
Research
Program
DRAFT
Overview

Objective
of
Biodegradation
Studies
for
Telomer­
based
Polymeric
Products

Analytical
Considerations
&
Limitations

Biodegradation
in
Sludge

Biodegradation
in
Soil

Summary
&
Conclusions
2003­
16­
09
,
page
3
Telomer
Research
Program
DRAFT
Study
Objective

Do
Telomer­
based
Polymeric
Products
(
TBPP)
biodegrade
to
PFOA?

TRP
recognizes
that
data
is
needed
to
inform
this
question
and
offers
a
study
approach
where
both
Telomer­
based
Polymeric
Products
and
Telomer­
based
Polymers
are
investigated
and
the
desire
for
timely
results.

Proposed
Studies

address
partitioning
and
biotransformation
in
relevant
environmental
compartments

start
with
laboratory
studies
that
are
simple
and
inform
the
question
of
whether
telomer­
based
polymeric
products
and
telomer­
based
polymers
have
the
potential
to
transform
to
PFOA
2003­
16­
09
,
page
4
Telomer
Research
Program
DRAFT
80%
Water
20%
Telomer
Polymer
°
Aqueous
Dispersion
of .

°
Polymeric
Particles
100­
200
nm
with...

°
Hydrocarbon
Surfactant(
s)

What
is
a
Typical
Telomer­
Based
Polymeric
Product's
Composition
?

Telomer
Polymeric
Product
Variables

wt.%
solids
in
product
(~
20%)

19.8
+
%
polymer

0.2
+
%
residual
raw
materials

wt.%
fluorine

wt.%
Telomer
raw
materials

wt.%
eight­
fluorinated
carbon
chain
C8F17­

PFOA
(
from
product
analysis)

Mol.
Wt.
­
Typically
>
10,000
Daltons

polyacrylates

polyurethanes
2003­
16­
09
,
page
5
Telomer
Research
Program
DRAFT
Release
of
Telomer­
based
polymeric
products

Telomer­
based
polymeric
products
(
TBPP)
primarily
enter
the
environment

in
sewage
treatment
plants
(
stp)

in
soil
via
sludge
amendment
to
agricultural
soils

in
surface
water
and
sediment
via
stp
e.
g.
sorbed
to
effluent
particles

in
landfills
from
sludge
or
disposal
of
treated
articles
(
carpets,
textiles,

paper)

TRP
Program
:

Sludge
and
Soil
are
environmental
compartments
for
TBPP
where
study
work
should
be
focused

Other
compartments
(
air,
sediment,
water)
are
...

considered
in
the
work
plans
for
soil
and
sludge
or
are
not
primary
compartments
of
entry
for
TBPP

considered
in
the
TRP
work
on
8­
2
Telomer
B
Alcohol
2003­
16­
09
,
page
6
Telomer
Research
Program
DRAFT
Analytical
Method
Requirements

First,
establishment
of
robust
analytical
methods
for
study
matrices
is
mandatory
to
achieve
meaningful
results

Matrices

sludge,
aerobic
and
anaerobic
soil;
appropriate
dispersion
of
test
polymer
solid

Analytes

e.
g.
Fluoride,
PFOA
and
Total
Organic
Fluorine
(
TOF)

Extraction
&
Recovery
Demonstration

analyte
recovery
within
test
time
period
must
be
acceptable

sludge
28
to
84
days

soil
4
­
6
months

It
is
required
by
test
guidelines
to
only
begin
testing
after
appropriate
analytical
methods
have
been
established
and
demonstrated.
2003­
16­
09
,
page
7
Telomer
Research
Program
DRAFT
Establish
Dispersion
Method
Establish
Extraction
Method
Establish
Quantification
Method
Quality
Check
Spiking
experiment
Full
Exposure
Period
Quality
Check
START
REAL
TEST
Test
method
not
applicable
yes
yes
no
no
It
has
to
be
proven,
for
the
study
to
be
conducted
 ..

°
that
dispersion,
extraction
and
quantification
is
possible
°
that
the
development
methodology
is
applicable
to
conditions
over
the
full
study
exposure
time
period
(
e.
g.

28d,
84d
or
6
months)

°
that
analyte
recovery
and
measurement
is
stable
over
the
study
time
period
Improvement
?
Analytical
Requirements
for
Environmental
Studies
­
General
Overview
2003­
16­
09
,
page
8
Telomer
Research
Program
DRAFT
Water
°
Fluoride
°
PFOA
Solids
°
Total
Fluorine
Air
Trap
°
Fluoride
°
PFOA
°
8­
2
TBA
+
+

Analysis
Matrices
Polymeric
Product
(
TBPP)

°
Inorganic
Fluoride
(
F­)

°
PFOA
?

°
8­
2
TBA
?

°
Total
Organic
Fluorine
How
to
achieve
Mass
Balance
The
measurements
fit
together
Solvent
Extraction
°
PFOA
°
8­
2
TBA
°
Other
organic
fluorine
compounds
as
TOF
Step
1
Characterization
of
TBPP
Test
Substance
Step
2
Analyte
Recovery
&
Quantitation
2003­
16­
09
,
page
9
Telomer
Research
Program
DRAFT
Sewage
Treatment
Plants
(
STP)

Biodegradability
Testing
Experimental
Design
Discussion
2003­
16­
09
,
page
10
Telomer
Research
Program
DRAFT
Test
Materials
for
STP
Biodegradation
Study
Proposal
9
Sept.
2003

OECD
302
B
(
Zahn­
Wellens
/
EMPA
Test)
on

Two
(
2)
Telomer­
based
Polymeric
Products
(
TBPP)
&
2
Telomer­
based
polymers
isolated
from
TBPP
Products
will
be
from
the
12
that
are
included
in
the
TRP
LOI

Two
isolated
polymers
from
the
two
Products

to
understand
whether
the
polymer
alone
undergoes
transformation

characterization
of
the
products
and
isolated
polymers
will
be
done

will
enable
method
development
and
demonstration
for
longer­
term
studies

provides
results
in
short
timeframe

Then
 ..
Conduct
302B
on
additional
10
polymeric
products
in
LOI

This
is
a
modification
of
the
TRP
LOI
commitment
2003­
16­
09
,
page
11
Telomer
Research
Program
DRAFT
Test
Materials
for
STP
Biodegradation
Study
Proposal
16
Sept.
2003

Alternatively
  ...
To
ensure
representativeness

We
propose
to
study

the
twelve
(
12)
TBPP
outlined
in
the
TRP
LOI

in
equal
weight
proportions,
as
a
composite

in
an
OECD
302B
Modified
Zahn­
Wellens
Study

and

the
isolated
polymers
from
the
twelve
(
12)
TBPP

in
equal
weight
proportions,
as
a
composite

in
an
OECD
302B
Modified
Zahn­
Wellens
Study
2003­
16­
09
,
page
12
Telomer
Research
Program
DRAFT
Test
Materials
for
STP
Biodegradation
Study
Proposals

In
parallel,
we
propose
to
develop
a
study
protocol
to
conduct
 

OPPTS
835.5045
"
Modified
SCAS
Test
For
Insoluble
and
Volatile
Chemicals"

need
to
develop
and
demonstrate
feasible
analytical
methods

on
the
composite
of
Isolated
Polymers
(
from
Telomer
Based
Polymer
Products)

we
want
to
discuss
the
decision
triggers
for
this
study

and
to
develop
the
appropriate
work
to
demonstrate
analytical
feasibility
2003­
16­
09
,
page
13
Telomer
Research
Program
DRAFT
Biodegradation
Testing
Strategy
Telomer­
Based
Polymer
Product
(
TBPP)
or
Composite
Isolated
Polymer
from
TBPP
or
Composite
Conduct
Modified
SCAS
Test
on
Isolated
Polymer
only*

Does
TBPP
Biodegrade?
Yes
No
Conduct
Modified
SCAS
Test
on
TBPP*
SCAS:

Analytical
Methods
work
?

STOP
Decision
:

1)
PFOA
or
F­
>
LOQ
2)
related
to
residuals
STOP
No
Yes
Modified
Zahn­

Wellens/
EMPA
Test
LOI
Modified
Zahn­

Wellens/
EMPA
Test
LOI
SCAS:

Analytical
Methods
work
?
Yes
No
*
Kinetic
Investigations
will
be
considered
after
reviewing
study
results
2003­
16­
09
,
page
14
Telomer
Research
Program
DRAFT
Proposal
for
Modification
of
Performance
of
Test:

Modified
SCAS
Test
(
OPPTS
835.5045)

Run
study
for
12
weeks

Collect
and
freeze
samples
daily
over
12
weeks

Analyze
samples
at
Day
0,
Weeks
4,
8,
and
12.

Will
look
for:

1)
Effluent
&
Sludge
:
Total
Organic
Fluorine,
Fluoride
ion

2)
Effluent
&
Sludge
solids
:
PFOA

3)
Volatility
Traps
:
Total
Organic
Fluorine,
Fluoride
ion,
PFOA,
8_
2
Telomer
B
Alcohol

If
2
&
3
PFOA
concentration
is
less
than
LOQ,
stop.

If
2
or
3
PFOA
concentration
is
greater
than
LOQ,
then
consider
further
studies
and
analyses.
2003­
16­
09
,
page
15
Telomer
Research
Program
DRAFT
Modification
of
OECD
307
Aerobic
and
Anaerobic
Transformations
in
Soil
Experimental
Design
Discussion
2003­
16­
09
,
page
16
Telomer
Research
Program
DRAFT
Test
Materials
for
Soil
Biodegradation
Study
Proposals

OECD
307
Aerobic
and
Anaerobic
Transformations
in
Soil

Two
(
2)
Telomer­
based
polymers
isolated
from
TBPP
Products
will
be
from
the
12
that
are
included
in
the
TRP
LOI

Two
isolated
polymers
from
the
two
Products

to
understand
whether
the
polymer
alone
undergoes
transformation

characterization
of
the
products
and
isolated
polymers
will
be
done

will
enable
method
development
and
demonstration

option
:
conduct
study
on
isolated
polymer
composite
2003­
16­
09
,
page
17
Telomer
Research
Program
DRAFT
Biodegradation
Testing
in
Soil
Testing
Strategy
Pilot
Study

Pilot
study
:
Modified
OECD
307
Test
setting

Establishment
and
Verification
of
the
Analytical
method
for
four
to
six
months
exposure

Testing
of
two
isolated
polymers

Use
of
the
OECD
307
(
Aerobic
and
anaerobic
transformation
in
soil)

setting

apply
aerobic
and
anaerobic
conditions

Alternatively,
conduct
study
on
isolated
polymer
composite

Kinetic
investigations

will
be
considered
after
reviewing
study
results
2003­
16­
09
,
page
18
Telomer
Research
Program
DRAFT
Work
Plan
Path
Forward
1.
Test
substance
characterization
2.
Develop
Analytics
for
Zahn­
Wellens,
Soil
and
SCAS
studies

methods
and
analytes
of
interest
3.
Commence
Zahn­
Wellens
as
soon
as
possible
4.
Develop
SCAS
Study
Proposal
5.
Develop
Soil
Study
Proposal
1
9/
12/
03
Detailed
Test
Protocol
Outline
Proposal,
September
12,
2003
1.
Introduction
The
overall
goal
of
this
program
is
to
determine
if
incineration
of
telomer­
based
substances
(
in
applications
where
incineration
is
a
commonly
used
disposal
practice)
is
a
potential
source
of
PFOA
to
the
environment.

This
document
presents
a
detailed
outline
of
a
protocol
for
a
research
program
to
conduct
incineration
testing.
Substantial
work
is
necessary
to
integrate
available
sampling
and
analytical
methods
for
PFOA
into
an
experimental
program
for
incineration
testing.

Following
agreement
on
this
document,
a
test
protocol
and
Quality
Assurance
Project
Plan
(
QAPP)
can
be
prepared.
The
QAPP
will
include
data
quality
objectives
(
DQOs).
Although
alternative
methods
are
included
herein
to
the
extent
practicable,
it
is
anticipated
that
the
administration
of
this
program
will
allow
for
obtaining
approval
to
modify
the
test
program
(
e.
g.,
to
substitute
alternate
test
methods)
in
case(
s)
where
proposed
method(
s)
do
not
appear
able
to
provide
information
meeting
these
DQOs.

The
QAPP
will
also
address
other
quality
assurance/
quality
control
elements
for
this
test
program,
including
project
organization,
chain
of
custody,
and
sample
container
selection.

Details
of
this
test
protocol
are
outlined
in
subsequent
sections.
The
test
objective
is
presented
in
Section
2.
Section
3
discusses
the
overall
experimental
approach
and
preliminary
testing
prior
to
the
combustion
tests.
Section
4
presents
the
materials
and
methods
involved
in
this
test
program
with
focus
on
combustion
testing.
Plans
for
sampling
and
analysis
are
described
in
Section
5.
Section
6
reviews
how
results
of
this
program
will
be
reported.

2.
Test
Objective
The
specific
objective
of
this
test
program
is
to
investigate
incineration
of
telomer­
based
substances
under
laboratory­
scale
conditions
representative
of
typical
2
9/
12/
03
municipal
waste
combustor
operations
in
the
U.
S.
to
quantitatively
determine
potential
emission
levels
of
PFOA.

3.
Experimental
Approach
Each
test
material
(
as
described
in
Section
4.2)
will
undergo
elemental
analysis
(
see
Section
5.2)
to
define
the
basic
parameters
for
stoichiometric
calculations.

Thermogravimetric
analysis
(
TGA)
per
ASTM
E1641
will
be
conducted
to
determine
the
gasification
temperature
of
each
test
material.
TGA
will
be
performed
on
each
sample
to
determine
the
temperature
range
required
for
gasification
of
the
sample
and
ash
content.
This
analysis
will
be
conducted
in
flowing
air
from
room
temperature
to
1000
°
C
at
25
°
C/
minute
using
3
to
5
mg
samples.
The
temperature
for
100%
gasification
for
each
test
material
will
be
considered
in
establishing
conditions
for
the
gasification
section
(
pyroprobe
section)
of
the
experimental
apparatus
for
the
combustion
tests;
see
section
4.3.

Overall,
stoichiometry
and
TGA
results
will
form
the
basis
for
setting
experimental
conditions
(
e.
g.,
time
and
temperature)
in
the
gasification
section
of
the
experimental
system
during
the
combustion
tests.

Combustion
tests
will
be
carried
out
at
specified
operating
conditions
as
presented
in
Section
4.3.

Prior
to
combustion
testing,
quantitative
transport
of
PFOA
will
be
verified.
For
these
transport
tests,
plans
call
for
gasifying
nominally
1
mg
of
PFOA
at
150
to
200
o
C
with
transfer
line
and
reactor
temperatures
nominally
30
to
50
o
C
higher
than
the
gasification
temperature.
The
exhaust
gas
will
be
sampled
and
analyzed
as
described
in
Section
5.1.4
to
determine
quantitation
of
PFOA.
If
the
PFOA
transport
efficiency
is
found
to
be
less
than
a
specified
level
(
e.
g.,
70%),
then
the
reactor
would
be
disassembled
and
extracted
with
an
appropriate
solvent
(
e.
g.,
methanol).
This
solvent
sample
would
be
analyzed
via
the
analytical
method
described
in
Section
5.1.4
to
determine
if
adsorption
on
the
reactor
walls
is
responsible
for
the
low
recovery.
The
experimental
apparatus
described
in
Section
4.1
is
configured
such
that
additional
extractions
of
the
transfer
lines
between
the
pyroprobe
and
the
reactor
and
3
9/
12/
03
between
the
reactor
and
the
downstream
sampling
point
are
not
feasible.

4.
Materials
and
Methods
4.1
Combustion
Test
Experimental
Apparatus
Incineration
testing
is
to
be
accomplished
using
a
batchcharged
continuous
flow
reactor
system.
The
test
sample
is
gasified
and
transported
to
a
high
temperature
reactor
In
the
high
temperature
reactor,
the
sample
vapors
are
subjected
to
controlled
conditions
of
residence
time,
temperature,
and
excess
air.
Combustion
products
are
collected
for
quantitative
analysis.

Use
of
the
Advanced
Thermal
Reactor
System
(
ATRS)
at
the
University
of
Dayton
Research
Institute
(
UDRI)
is
planned.
A
schematic
of
the
ATRS
as
planned
for
use
in
this
test
program
is
presented
in
Figure
1.

Figure
1.
Schematic
of
ATRS
for
Planned
Testing
Gas
Chromatograph
Mass
Selective
Detector
Workstation
Reactor
Coolant
Cold
Trap
Pyroprobe
Inlets
&
Main
Gas
Flow
Supplemental
Gas
Flow
To
Ventilation
System
Bubblers
4
9/
12/
03
Supplemental
gas
flow
and
main
gas
flow
refer
to
the
planned
gas
feeds
(
synthetic
air
and
methane).

The
ATRS
consists
of
a
reactor
assembly
and
in­
line
gas
chromatograph/
detector
system
connected
via
a
cryogenic
interface.
The
reactor
assembly
consists
of
a
thermally
insulated
enclosure
housing
the
sample
introduction,
reactor,
and
transfer
line
systems.
Sample
introduction
for
solid
materials
employs
a
pyroprobe,
a
device
designed
to
gasify
samples
by
heating
them
at
a
fixed
rate.
During
combustion
tests,
the
transfer
line
between
the
pyroprobe
and
the
reactor
is
heated
and
maintained
above
250
oC.
The
reactor
is
housed
within
its
own
small
tube
furnace
and
may
be
independently
heated
to
as
high
as
1200
oC.
(
Actual
conditions
planned
for
this
test
program
are
presented
in
Section
4.3.)
The
exhaust
line
from
the
reactor
is
heat
traced
to
prevent
cool
regions
where
reactor
products
could
otherwise
be
lost
through
condensation.
The
cryogenic
interface
(
cold
trap)
is
of
a
shell
and
tube
design
and
provides
significant
cooling
of
the
combustion
exhaust
gas
prior
to
on­
line
monitoring
or
sample
collection.

For
this
test
program,
plans
call
for
setting
the
cold
trap
temperature
at
nominally
 
15
oC
to
be
below
the
freezing
point
of
water
(
H2O)
but
above
the
sublimation
temperature
of
carbon
dioxide
(
CO2)
to
assist
in
separating
H2O
from
carbon
monoxide
(
CO)
and
CO2.

The
in­
line
gas
chromatograph
(
with
molecular
sieve
column)
and
mass
selective
detector
(
MSD)
are
planned
to
be
used
to
monitor
CO
and
CO2.
Exhaust
gas
samples
for
off­
line
analysis
will
be
collected
from
the
vent
line
off
the
cold
trap;
see
Section
5.1.

4.2
Test
Materials
Two
test
materials
are
planned
for
this
study:

 
A
single
representative
composite
mixture
of
the
LOI
telomer­
based
polymeric
products
which
are
applied
to
paper,
as
solids,
in
equal
proportions.

 
A
single
representative
composite
mixture
of
the
LOI
telomer­
based
polymeric
products
which
are
applied
to
textiles,
as
solids,
in
equal
proportions.
5
9/
12/
03
4.3
Combustion
Test
Experimental
Conditions
The
test
materials
described
in
Section
4.2
will
be
subjected
to
laboratory­
scale
incineration
using
the
experimental
apparatus
described
in
Section
4.1.

Synthetic
air
(
mixture
of
21%
oxygen
and
79
%
nitrogen)
will
be
used
in
place
of
compressed
air
to
prevent
potential
interference
in
the
experimental
system
due
to
background
levels
of
CO2
in
compressed
air.

Methane
will
be
used
as
needed
as
a
supplemental
fuel
to
ensure
the
presence
of
sufficient
hydrogen
to
convert
fluorine
to
hydrogen
fluoride
(
HF).

Two
levels
of
temperature
for
the
high
temperature
reactor
are
planned:

 
900
°
C
 
1000
o
C
As
the
Appendix
indicates,
the
lower
temperature
represents
the
low
end
of
normal
operating
temperatures
for
the
high
temperature
zone
of
municipal
waste
combustors
(
MWCs)
in
the
U.
S.,
and
the
higher
temperature
represents
the
typical
operating
temperature
for
the
high
temperature
zone
of
MWCs
and
medical
waste
incinerators
in
the
U.
S.

At
each
temperature
level,
the
planned
operating
conditions
for
the
high
temperature
reactor
during
the
combustion
tests
are
2
seconds
gas
residence
time
and
10%
oxygen
in
the
exhaust
gas.
As
the
Appendix
indicates,
these
conditions
are
representative
of
typical
operating
conditions
for
MWCs
in
the
U.
S
As
noted
in
Table
1,
three
replicates
are
planned
for
each
test
level
(
combination
of
test
material
and
temperature).

Table
1
Test
Material
Paper
composite
Paper
composite
Textile
composite
Textile
composite
Temperature
900
o
C
1000
o
C
900
o
C
1000
o
C
No.
of
runs
3
3
3
3
Additionally,
at
least
one
thermal
blank
(
with
combustion
test
feeds
except
for
the
test
material)
is
planned
for
each
group
of
3
runs.
6
9/
12/
03
The
amount
of
test
material
fed
will
be
large
enough
to
assure
ability
to
detect
PFOA
in
the
emissions,
but
small
enough
to
assure
sufficient
excess
oxygen
to
be
representative
of
typical
MWC
conditions.
While
elemental
analysis
and
TGA
is
required
to
establish
the
planned
mass
of
sample,
the
expected
sample
size
is
on
the
order
of
1
to
2
mg.

The
temperature
in
the
pyroprobe
section
will
be
maintained
at
approximately
50
to
100
o
C
above
the
highest
temperature
for
100%
gasification
across
the
test
materials
as
determined
from
the
thermogravimetric
experiments
earlier
in
the
test
program.
This
is
necessary
to
assure
complete
gasification
of
the
sample
of
test
material
and
a
common
set
of
experimental
conditions
across
the
test
materials
during
combustion
testing.

5.
Combustion
Test
Sampling
and
Analysis
5.1
Exhaust
Gas
Sampling
&
Analysis
Gas
samples
for
off­
line
analysis
will
be
collected
from
a
vent
line
off
the
cold
trap
and
may
be
subjected
to
additional
external
cooling
(
e.
g.,
ice
bath)
as
needed.

Analysis
of
the
exhaust
gas
samples
of
the
thermal
blanks
will
focus
on
PFOA
since
the
primary
purpose
of
conducting
these
blank
runs
is
to
check
for
possible
crosscontamination
between
sample
runs.

5.1.1
Monitored
Parameters
As
noted
in
Section
4.1,
on­
line
monitoring
for
CO
and
CO2
via
the
in­
line
GC
using
a
molecular
sieve
column
and
MSD
is
planned.
Alternately,
Tedlar
®
bag
samples
of
exhaust
gas
may
be
collected
for
off­
line
CO
and
CO2
analysis.

Exhaust
gas
flow
rate
will
be
monitored
based
on
measured
input
flow
rates
of
the
synthetic
air
and
methane
gas
feeds.
Exhaust
gas
oxygen
concentration
will
be
calculated,
based
on
measured
input
flow
rate
of
synthetic
air
and
methane
assuming
complete
combustion.
7
9/
12/
03
5.1.2.
Fluoride
The
exhaust
gas
will
be
sampled
and
analyzed
for
fluoride
ion
to
assist
in
performing
a
fluoride
balance
across
the
experimental
system.

Fluoride
ion
will
be
sampled
via
absorption
into
aqueous
solution,
using
bubblers
(
low
pressure
drop
midget
impingers)
in
series.
As
Figure
1
indicates,
initial
plans
call
for
using
three
bubblers
in
series
with
the
first
one
empty
to
serve
as
a
knock­
out
pot
and
the
second
and
third
containing
a
predetermined
amount
of
aqueous
solution.
(
The
number
of
aqueous
solution
bubblers
will
be
adjusted
as
necessary.)
Upon
completion
of
sample
collection,
the
amounts
in
each
bubbler
will
be
measured
and
the
contents
of
the
bubblers
will
be
quantitatively
transferred
into
a
container
for
subsequent
analysis
for
total
inorganic
fluorine
(
i.
e.,
fluoride
ion)
via
ion
chromatography
or
ion
selective
electrode.

5.1.3
Total
Fluorine
The
aqueous
solution
sample
collected
as
described
in
Section
5.1.2
is
also
planned
to
be
subjected
to
analysis
for
total
fluorine
via
Wickbold
torch
so
that
total
organic
fluorine
can
be
determined
by
difference
between
total
fluorine
and
total
inorganic
fluorine.
Work
is
in
progress
to
confirm
that
detection
limits
for
total
fluorine
analysis
via
Wickbold
torch
are
low
enough
to
be
informative
for
this
test
system.

5.1.4
PFOA
Exhaust
gas
samples
will
be
analyzed
for
PFOA
via
LC/
MS/
MS
at
a
qualified
commercial
laboratory
operating
under
suitable
data
quality
guidelines.

Development
is
in
progress
to
define
the
most
suitable
sampling
technique
for
PFOA
in
the
incineration
exhaust
gas.

Initial
plans
call
for
using
the
aqueous
solution
bubblers
described
in
Section
5.1.2
to
collect
PFOA
from
the
exhaust
gas
and
for
sending
a
portion
of
the
aqueous
solution
for
PFOA
analysis
as
described
above.
Additionally,
an
attempt
will
be
made
to
use
an
OSHA
Versatile
Sampler
(
OVS)
as
a
back­
up
sampling
device.
If
OVS
is
also
used
to
sample
8
9/
12/
03
PFOA
in
the
exhaust
gas,
then
the
OVS
would
also
be
sent
for
off­
line
LC/
MS/
MS
analysis
to
quantify
PFOA
as
a
crosscheck
on
the
aqueous
solution
bubbler
results.

5.2
Test
Material
Sampling
&
Analysis
Each
test
material
composite
will
be
dissolved
in
an
appropriate
solvent
and
analyzed
for
PFOA
via
LC/
MS/
MS
at
a
qualified
commercial
laboratory
operating
under
suitable
data
quality
guidelines.

As
noted
in
Section
3,
each
test
material
composite
will
undergo
elemental
analysis
for
carbon,
hydrogen,
nitrogen,
fluorine,
sulfur,
and
oxygen
by
difference.
Ultimate
analysis
(
ASTM
D3176
and
other
ASTM
methods
referenced
therein)
are
planned
for
this
analysis.
Moisture
is
also
determined
by
this
method.
Depending
on
sample
size,
it
may
be
necessary
to
implement
the
microanalytic
analog
of
ultimate
analysis.

In
order
to
enable
determination
total
organic
fluoride
(
in
each
test
material
composite)
by
difference
between
fluorine
(
total
fluorine)
and
fluoride
(
total
inorganic
fluoride),
each
test
material
will
undergo
aqueous
extraction
and
analysis
of
the
aqueous
extract
for
fluoride
ion
(
via
ion
chromatography
or
ion
selective
electrode)
to
yield
a
total
inorganic
fluorine.

6.
Reporting
of
Results
6.1
Exhaust
Gas
Results
6.1.1
Monitored
Parameters
CO
will
be
reported
in
terms
of
parts
per
million
by
volume
(
ppmv).
CO
2
will
be
reported
in
terms
of
percent
by
volume
(%).
Oxygen
will
be
reported
in
terms
of
percent
by
volume
(%).
Exhaust
gas
flowrate
will
be
reported
in
units
of
cubic
centimeters
per
minute
(
cm
3/
min).

6.1.2
Fluoride
and
Fluorine
Total
fluorine
and
fluoride
(
total
inorganic
fluorine)
in
the
exhaust
gas
will
each
be
reported
in
terms
of
concentration
(
mass
of
fluorine
per
volume
of
exhaust
gas)
9
9/
12/
03
in
the
gas
as
well
as
on
the
basis
of
mass
of
fluorine
per
mass
of
starting
test
material.

Total
organic
fluorine
will
be
determined
by
difference
between
total
fluorine
and
total
inorganic
fluorine.

6.1.3
PFOA
PFOA
in
the
exhaust
gas
will
be
reported
in
terms
of
concentration
in
the
gas
as
well
as
on
the
basis
of
mass
per
mass
of
starting
test
material.

6.2
Test
Material
Results
PFOA
for
each
composite
will
be
reported
in
terms
of
mass
per
mass
of
composite
feed
material.

Elemental
compositions
and
total
organic
fluoride
will
be
reported
in
terms
of
mass
per
mass
of
composite
feed
material.

6.3
Exposure
Assessment
In
the
event
that
PFOA
is
found
in
the
exhaust
gas
at
a
concentration
above
the
limit
of
quantitation
(
for
the
matrix)
from
one
or
more
experiments
described
in
this
protocol,
then
the
potential
for
exposure
related
to
incineration
of
the
subject
material
will
be
assessed
to
inform
the
basis
for
possible
next
steps.

This
assessment
will
consider
a
number
of
factors
such
as
 
Test
program­
determined
PFOA
emission
factor,

 
Estimated
amounts
of
subject
material
in
feed
to
fullscale
waste
incinerators,
and
 
Degree
of
post­
combustion
air
pollution
control
(
e.
g.,
use
and
effectiveness
of
carbon
adsorption).
10
9/
12/
03
Appendix
Polymers
of
the
sort
being
investigated
in
this
test
program
may
be
present
at
trace
to
low
concentrations
in
municipal
solid
waste
or
in
medical
waste
and
therefore
may
be
incinerated.

A.
1
Types
of
Incinerators
A.
1.1
Municipal
Waste
Combustors
According
to
the
Integrated
Waste
Services
Association
(
IWSA),
there
are
a
total
of
98
waste­
to­
energy
facilities
operating
municipal
waste
combustors
(
MWCs)
in
the
U.
S.
as
of
2002.(
IWSA
2002)
Table
A­
1
summarizes
the
number
and
annual
capacity
of
these
units
by
type
of
technology
employed.

Table
A­
1.
MWCs
in
2002
Type
Number
of
Facilities
Annual
Capacity
(
million
Ton/
year
Mass
Burn
68
22.5
Refused
Derived
Fuel
(
RDF)
18
6.4
Modular
12
0.5
Total
98
29.4
As
the
capacity
values
indicate,
modular
units
are
generally
small
MWCs
accounting
for
less
than
a
total
of
2%
of
the
municipal
solid
waste
incinerated
in
the
U.
S.
in
2002.

A.
1.2
Hospital/
Medical/
Infectious
Waste
Incinerators
Although
earlier
reports
indicated
over
2200
medical
waste
incinerators
in
the
U.
S.
in
the
1990s
(
EPA
2000a),
the
current
EPA
Office
of
Air
Quality,
Planning,
and
Standards
(
OAQPS)
inventory
indicates
that
there
are
116
hospital/
medical/
infectious
waste
incinerators
(
HMIWIs)
in
the
U.
S.
as
of
July
28,
2003.
(
EPA
2003)

This
represents
a
greater
than
90%
reduction
in
the
number
of
operating
HMIWIs
in
the
U.
S.
Many
medical
waste
incinerators
were
closed
rather
than
upgraded
to
meet
new
emission
standards,
as
hospitals
improved
their
programs
to
segregate
infectious
("
red
bag")
waste
burned
in
HMIWIs
11
9/
12/
03
from
non­
infectious
("
black
bag")
waste
handled
as
municipal
solid
waste
after
it
leaves
the
hospital.

A.
2
Operating
Conditions
As
noted
by
EPA,
many
incinerators
for
municipal
solid
waste
are
designed
to
operate
in
the
combustion
zone
at
1800
°
F
[
982
°
C]
to
2000
°
F
[
1093
°
C]
to
ensure
good
combustion.
(
EPA
1995)
EPA
new
source
performance
standards
(
NSPS)
and
emission
guidelines
for
both
municipal
waste
combustors
(
MWCs)
and
hospital/
medical/
infectious
waste
incinerators
(
HMIWIs)
are
based
on
the
use
of
"
good
combustion
practices"
(
GCP).
(
EPA
1997,
EPA
2000b,
EPA
2000c,
Van
Remmen
1998)

Speaking
of
MWCs,
Donnelly
notes,
"
Design
of
modern
efficient
combustors
is
such
that
there
is
adequate
turbulence
in
the
flue
gas
to
ensure
good
mixing,
a
hightemperature
zone
(
greater
than
1000
o
C)
to
complete
burnout,
and
long
enough
residence
time
at
high
temperature
(
1­
2
sec)
for
complete
burnout."
(
Donnelly
2000)
The
term
"
flue
gas"
here
refers
to
the
gas
above
the
grate.

With
respect
to
HMIWIs,
Van
Remmen
states
"
any
unit
which
presently
[
prior
to
compliance
date]
has
a
[
secondary
chamber]
residence
time
less
than
two
seconds
at
1000
o
C
does
not
meet
the
requirement
for
good
combustion
under
the
new
regulations."
(
Van
Remmen
1998)

Similarly,
most
MWCs
are
expected
to
typically
operate
with
a
2
second
gas
residence
time
in
the
high
temperature
zone
in
order
to
assure
compliance
with
emission
standards
on
carbon
monoxide
and
dioxins.

A.
2.1
MWC
Operating
Conditions
EPA
presents
operating
data
for
some
MWCs
in
"
Municipal
Waste
Combustion
Assessment:
Technical
Basis
for
Good
Combustion
Practice"
and
points
the
reader
elsewhere
for
additional
data
on
specific
representative
MWCs.

Modular
MWC
Specifically,
this
background
document
(
EPA
1989)
includes
secondary
chamber
temperatures
for
modular
MWCs
that
had
CO
emission
levels
less
than
current
emission
standards,
and
these
are
summarized
in
Table
A­
2.
12
9/
12/
03
Table
A­
2.
Modular
MWC
Temperatures
Secondary
Chamber
Temperature
(
o
C)
Oswego
Co.,
NY
Red
Wing,
MN
Start
of
campaign
1012
Mid­
range
secondary
temperature
951
End
of
campaign
995
Low
secondary
temperature
885
Mean
secondary
temperature
954
­
1071
As
highlighted
in
Table
A­
2,
typical
secondary
chamber
temperatures
for
these
dual­
chamber
modular
units
are
in
the
range
of
951
to
1071
o
C.

As
indicated
in
section
A.
1,
such
modular
units
are
generally
small
MWCs
and
account
for
less
than
a
total
of
2%
of
the
municipal
solid
waste
incinerated
in
the
U.
S.

Although
this
1989
EPA
background
document
does
not
present
temperature
data
for
mass
burn
nor
RDF
units,
reports
from
the
National
Incinerator
Testing
and
Evaluation
Program
(
NITEP)
present
operating
data
for
an
RDF
combustor
(
Mid­
Connecticut)
and
for
a
mass
burn
waterwall
combustor
(
Quebec
City)
otherwise
discussed
in
the
1989
background
document.

RDF
MWC
Furnace
temperatures
and
flue
gas
oxygen
levels
for
Mid­
Connecticut
RDF
combustor
performance
tests
operating
under
good
combustion
conditions
across
a
range
of
steam
loads
(
Finklestein
and
Klicius
1994)
are
summarized
in
Table
A­
3.

Table
A­
3.
RDF
MWC
 
Mid­
Connecticut
Steam
load
Low
low
Intermediate
Intermediate
normal
normal
normal
high
test
number
PT­
13
PT­
14
PT­
10
PT­
02
PT­
09
PT­
08
PT­
11
PT­
12
Furnace
temperature
(
o
C)
965
1004
1012
1022
1033
1015
1026
1049
flue
gas
O
2
(%)
10.1
9.6
9.2
9.1
7.6
7.5
7.9
6.4
The
average
operating
conditions
for
this
RDF
unit
across
the
range
of
steam
loads
are
1016
o
C
and
8.4%
O
2.

Mass
Burn
MWC
Furnace
temperatures
(
average
of
front
and
rear
radiation
chamber
temperatures)
and
flue
gas
oxygen
levels
(
dry
basis)
for
Quebec
City
mass
burn
combustor
performance
tests
operating
under
good
combustion
conditions
across
a
13
9/
12/
03
range
of
steam
loads
(
Environment
Canada
1988)
are
summarized
in
Table
A­
4.

Table
A­
4.
Mass
Burn
MWC
 
Quebec
City
Steam
load
Low
low
Low
design
design
Design
High
high
test
number
PT02
PT10
PT11
PT05
PT06
PT12
PT07
PT09
Furnace
temperature
(
o
C)
849
875
869
1014
1030
992
1085
1006
flue
gas
O
2
(
dry)
13
13
12
9
9
10
10
10
The
average
operating
conditions
for
this
mass
burn
unit
across
the
range
of
steam
loads
are
965
o
C
and
10.8%
O
2.
When
operated
at
design
steam
load,
the
average
operating
conditions
for
this
mass
burn
MWC
are
1012
o
C
and
9.3%
O
2.

MWC
Summary
Considering
the
relative
quantities
of
municipal
waste
burned
annually
in
each
type
of
MWC
and
the
data
in
this
section,
average
typical
operating
conditions
for
the
high
temperature
zone
of
MWCs
are
nominally
1000
o
C
and
10%
O
2.

A.
2.2
HMIWI
Operating
Conditions
EPA
notes
that
over
97%
of
medical
waste
incinerators
are
controlled
air
modular
units
(
EPA
2000a).
Recent
communication
with
EPA
OAQPS
indicates
that
virtually
all
existing
HMIWIs
are
controlled
air
modular
(
two­
chamber)
units.

Theodore
reports
the
range
of
temperatures
for
the
secondary
chamber
of
controlled
air
medical
waste
incinerators
as
980
to
1200
o
C.
(
Theodore
1990)
EPA
notes
that
auxiliary
fuel
(
e.
g.,
natural
gas)
is
burned
in
the
secondary
chamber
of
medical
waste
incinerators
to
sustain
temperatures
in
the
range
of
985
to
1095
o
C
and
that
combustion
air
at
100
to
300
%
in
excess
of
the
stoichiometric
requirement
is
usually
added
to
the
secondary
chamber.
(
EPA
2000a)

As
noted
above,
a
more
recent
report
indicates
that
existing
HMIWIs
operate
with
secondary
chamber
temperatures
greater
than
or
equal
to
1000
oC
with
a
gas
residence
of
2
seconds.
(
Van
Remmen
1998)
14
9/
12/
03
References
Donnelly,
J.
R.
Waste
Incineration
Sources:
Municipal
Waste
Combustion.
In:
W.
T.,
ed.,
Air
Pollution
Engineering
Manual,
2nd
edition.
Air
and
Waste
Management
Association.
New
York,
NY:
Van
Nostrand
Reinhold,
2000,
pp
257­
268.

Environment
Canada.
National
Incinerator
Testing
and
Evaluation
Program:
Environmental
Characterization
of
Mass
Burning
Incinerator
Technology
at
Quebec
City
 
Summary
Report,
EPS
3/
UP/
5,
June
1988.

Environmental
Protection
Agency
(
EPA).
Municipal
Waste
Combustion
Assessment:
Technical
Basis
for
Good
Combustion
Practice,
EPA
600/
8­
89­
063,
August
1989.

EPA.
Emission
Factor
Documentation
for
AP­
42
Section
2.1,
Refuse
Combustion,
May
1993.

EPA.
Decision
Maker's
Guide
to
Solid
Waste
Management,
Volume
II,
Chapter
8,
1995.

EPA.
Standards
of
Performance
for
New
Stationary
Sources
and
Emission
Guidelines
for
Existing
Sources:
Hospital/
Medical/
Infectious
Waste
Incinerators,
62
Federal
Register
48346,
September
15,
1997.

EPA.
Exposure
and
Human
Health
Reassessment
of
2,3,7,8­
Tetrachlorodibenzo­
p­
Dioxin
(
TCDD)
and
Related
Compounds,
Part
I:
Estimating
Exposure
to
Dioxin­
Like
Compounds
Volume
2:
Sources
of
Dioxin­
Like
Compounds
in
the
United
States,
Chapter
3,
EPA/
600/
P­
00/
001Bb,
Draft
Final
Report,
September
2000.

EPA.
New
Source
Performance
Standards
for
New
Small
Municipal
Waste
Combustion
Units,
65
Federal
Register
76350,
December
6,
2000.

EPA.
Emission
Guidelines
for
Existing
Small
Municipal
Waste
Combustion
Units,
65
Federal
Register
76378,
December
6,
2000.

EPA.
HMIWI
Facility
and
Emissions
Inventory,
draft,
July
28,
2003,
www.
epa.
gov/
ttnatw01/
129/
hmiwi/
2003hmiwi_
inventory.
xls
15
9/
12/
03
Finklestein,
A.
and
R.
D.
Klicius.
National
Incinerator
Testing
and
Evaluation
Program:
The
Environmental
Characterization
of
Refuse­
derived
Fuel
(
RDF)
Combustion
Technology,
Mid­
Connecticut
Facility,
Hartford,
Connecticut,
EPA­
600/
R­
94­
140
(
NTIS
PB96­
153432),
December
1994.

Integrated
Waste
Services
Association
(
IWSA).
The
2002
IWSA
Directory
of
Waste­
to­
Energy
Plants,
2002,
www.
wte.
org/
2002_
directory/
IWSA_
2002_
Directory.
html
Theodore,
L.
Air
Pollution
Control
and
Waste
Incineration
for
Hospitals
and
Other
Medical
Facilities,
Van
Nostrand
Reinhold,
New
York,
1990,
pp
313­
320.

Van
Remmen,
T.
Evaluation
of
the
available
air
pollution
control
technologies
for
achievement
of
the
MACT
requirements
in
the
newly
implemented
new
source
performance
standards
(
NSPS)
and
emission
guidelines
(
EG)
for
hospital
and
medical/
infectious
waste
incinerators,
Waste
Management,
1998,
Vol.
18,
pp
393­
402
Detailed
Test
Protocol
Outline
Proposal,
September
12,
2003
1.
Introduction
The
overall
goal
of
this
program
is
to
determine
if
incineration
of
fluoropolymers
(
in
applications
where
incineration
is
a
commonly
used
disposal
practice)
is
a
potential
source
of
PFOA
to
the
environment.

This
document
presents
a
detailed
outline
of
a
protocol
for
a
research
program
to
conduct
incineration
testing.
Substantial
preparatory
work
is
necessary
to
integrate
available
sampling
and
analytical
methods
for
PFOA
into
an
experimental
program
for
incineration
testing.

Following
agreement
on
this
document,
a
test
protocol
and
Quality
Assurance
Project
Plan
(
QAPP)
can
be
prepared.
The
QAPP
will
include
data
quality
objectives
(
DQOs).
Although
alternative
methods
are
included
herein
to
the
extent
practicable,
it
is
anticipated
that
the
administration
of
this
program
will
allow
for
obtaining
approval
to
modify
the
test
program
(
e.
g.,
to
substitute
alternate
test
methods)
in
case(
s)
where
proposed
method(
s)
do
not
appear
able
to
provide
information
meeting
these
DQOs.

The
QAPP
will
also
address
other
quality
assurance/
quality
control
elements
for
this
test
program,
including
project
organization,
chain
of
custody,
and
sample
container
selection.

Details
of
this
test
protocol
are
outlined
in
subsequent
sections.
The
test
objective
is
presented
in
Section
2.
Section
3
discusses
the
overall
experimental
approach
and
preliminary
testing
prior
to
the
combustion
tests.
Section
4
presents
the
materials
and
methods
involved
in
this
test
program
with
focus
on
combustion
testing.
Plans
for
sampling
and
analysis
are
described
in
Section
5.
Section
6
reviews
how
results
of
this
program
will
be
reported.

2.
Test
Objective
The
specific
objective
of
this
test
program
is
to
investigate
incineration
of
designated
fluoropolymers
under
laboratory­
scale
conditions
representative
of
typical
1
9/
12/
03
municipal
waste
combustor
operations
in
the
U.
S.
to
quantitatively
determine
emission
levels
of
PFOA.

3.
Experimental
Approach
Each
test
material
(
as
described
in
Section
4.2)
will
undergo
elemental
analysis
(
see
Section
5.2)
to
define
the
basic
parameters
for
stoichiometric
calculations.

Thermogravimetric
analysis
(
TGA)
per
ASTM
E1641
will
be
conducted
to
determine
the
gasification
temperature
of
each
test
material.
TGA
will
be
performed
on
each
sample
to
determine
the
temperature
range
required
for
gasification
of
the
sample
and
ash
content.
This
analysis
will
be
conducted
in
flowing
air
from
room
temperature
to
1000
°
C
at
25
°
C/
minute
using
3
to
5
mg
samples.
The
temperature
for
100%
gasification
for
each
test
material
will
be
considered
in
establishing
conditions
for
the
gasification
section
(
pyroprobe
section)
of
the
experimental
apparatus
for
the
combustion
tests;
see
section
4.3.

Overall,
stoichiometry
and
TGA
results
will
form
the
basis
for
setting
experimental
conditions
(
e.
g.,
time
and
temperature)
in
the
gasification
section
of
the
experimental
system
during
the
combustion
tests.

Combustion
tests
will
be
carried
out
at
specified
operating
conditions
as
presented
in
Section
4.3.

Prior
to
combustion
testing,
quantitative
transport
of
PFOA
will
be
verified.
For
these
transport
tests,
plans
call
for
gasifying
nominally
1
mg
of
PFOA
at
150
to
200
o
C
with
transfer
line
and
reactor
temperatures
nominally
30
to
50
o
C
higher
than
the
gasification
temperature.
The
exhaust
gas
will
be
sampled
and
analyzed
as
described
in
Section
5.1.4
to
determine
quantitation
of
PFOA.
If
the
PFOA
transport
efficiency
is
found
to
be
less
than
a
specified
level
(
e.
g.,
70%),
then
the
reactor
would
be
disassembled
and
extracted
with
an
appropriate
solvent
(
e.
g.,
methanol).
This
solvent
sample
would
be
analyzed
via
the
analytical
method
described
in
Section
5.1.4
to
determine
if
adsorption
on
the
reactor
walls
is
responsible
for
the
low
recovery.
The
experimental
apparatus
described
in
Section
4.1
is
configured
such
that
additional
extractions
of
the
transfer
lines
between
the
pyroprobe
and
the
reactor
and
2
9/
12/
03
between
the
reactor
and
the
downstream
sampling
point
are
not
feasible.

4.
Materials
and
Methods
4.1
Combustion
Test
Experimental
Apparatus
Incineration
testing
is
to
be
accomplished
using
a
batchcharged
continuous
flow
reactor
system.
The
test
sample
is
gasified
and
transported
to
a
high
temperature
reactor
In
the
high
temperature
reactor,
the
sample
vapors
are
subjected
to
controlled
conditions
of
residence
time,
temperature,
and
excess
air.
Combustion
products
are
collected
for
quantitative
analysis.

Use
of
the
Advanced
Thermal
Reactor
System
(
ATRS)
at
the
University
of
Dayton
Research
Institute
(
UDRI)
is
planned.
A
schematic
of
the
ATRS
as
planned
for
use
in
this
test
program
is
presented
in
Figure
1.

Figure
1.
Schematic
of
ATRS
for
Planned
Testing
Gas
Chromatograph
Mass
Selective
Detector
Workstation
Reactor
Coolant
Cold
Trap
Pyroprobe
Inlets
&
Main
Gas
Flow
Supplemental
Gas
Flow
To
Ventilation
System
Bubblers
3
9/
12/
03
Supplemental
gas
flow
and
main
gas
flow
refer
to
the
planned
gas
feeds
(
synthetic
air
and
methane).

The
ATRS
consists
of
a
reactor
assembly
and
in­
line
gas
chromatograph/
detector
system
connected
via
a
cryogenic
interface.
The
reactor
assembly
consists
of
a
thermally
insulated
enclosure
housing
the
sample
introduction,
reactor,
and
transfer
line
systems.
Sample
introduction
for
solid
materials
employs
a
pyroprobe,
a
device
designed
to
gasify
samples
by
heating
them
at
a
fixed
rate.
During
combustion
tests,
the
transfer
line
between
the
pyroprobe
and
the
reactor
is
heated
and
maintained
above
250
oC.
The
reactor
is
housed
within
its
own
small
tube
furnace
and
may
be
independently
heated
to
as
high
as
1200
oC.
(
Actual
conditions
planned
for
this
test
program
are
presented
in
Section
4.3.)
The
exhaust
line
from
the
reactor
is
heat
traced
to
prevent
cool
regions
where
reactor
products
could
otherwise
be
lost
through
condensation.
The
cryogenic
interface
(
cold
trap)
is
of
a
shell
and
tube
design
and
provides
significant
cooling
of
the
combustion
exhaust
gas
prior
to
on­
line
monitoring
or
sample
collection.

For
this
test
program,
plans
call
for
setting
the
cold
trap
temperature
at
nominally
 
15
oC
to
be
below
the
freezing
point
of
water
(
H2O)
but
above
the
sublimation
temperature
of
carbon
dioxide
(
CO2)
to
assist
in
separating
H2O
from
carbon
monoxide
(
CO)
and
CO2.

The
in­
line
gas
chromatograph
(
with
molecular
sieve
column)
and
mass
selective
detector
(
MSD)
are
planned
to
be
used
to
monitor
CO
and
CO2.
Exhaust
gas
samples
for
off­
line
analysis
will
be
collected
from
the
vent
line
off
the
cold
trap;
see
Section
5.1.

4.2
Test
Materials
Four
test
materials
are
planned
for
this
study.
Each
will
be
a
composite
mixture
of
representative
fluoropolymers,
as
solids,
in
equal
proportions
across
producers
for
each
of
the
following
four
classes:

 
Dry
melt
resins
(
FEP,
PFA,
THV,
ETFE,
HTE)
 
PTFE
 
Fluoroelastomers
 
Aqueous
dispersions
(
PTFE,
FEP,
PFA,
THV)

4
9/
12/
03
4.3
Combustion
Test
Experimental
Conditions
The
test
materials
described
in
Section
4.2
will
be
subjected
to
laboratory­
scale
incineration
using
the
experimental
apparatus
described
in
Section
4.1.

Synthetic
air
(
mixture
of
21%
oxygen
and
79
%
nitrogen)
will
be
used
in
place
of
compressed
air
to
prevent
potential
interference
in
the
experimental
system
due
to
background
levels
of
CO2
in
compressed
air.

Methane
will
be
used
as
needed
as
a
supplemental
fuel
to
ensure
the
presence
of
sufficient
hydrogen
to
convert
fluorine
to
hydrogen
fluoride
(
HF).

The
planned
operating
conditions
for
the
high
temperature
reactor
during
the
combustion
tests
are
900
°
C
with
2
seconds
gas
residence
time
and
10%
oxygen
in
the
exhaust
gas.
As
the
Appendix
indicates,
these
conditions
are
representative
of
typical
operating
conditions
for
the
high
temperature
zone
of
municipal
waste
combustors
(
MWCs)
in
the
U.
S.,
except
that
the
planned
temperature
reflects
the
low
end
of
normal
MWC
operating
temperatures.
Also,
as
the
information
in
the
Appendix
indicates,
the
planned
temperature
is
less
than
typical
secondary
chamber
operating
temperatures
for
medical
waste
incinerators
in
the
U.
S.

As
noted
in
Table
1,
three
replicates
are
planned
for
each
test
level
(
combination
of
test
material
and
temperature).

Table
1
Test
Material
Dry
melt
resin
composite
PTFE
composite
Fluoroelastomer
composite
Aqueous
dispersion
composite
Temperature
900
o
C
900
o
C
900
o
C
900
o
C
No.
of
runs
3
3
3
3
Additionally,
at
least
one
thermal
blank
(
with
combustion
test
feeds
except
for
the
test
material)
is
planned
for
each
group
of
3
runs.

The
amount
of
test
material
fed
will
be
large
enough
to
assure
ability
to
detect
PFOA
in
the
emissions,
but
small
enough
to
assure
sufficient
excess
oxygen
to
be
representative
of
typical
MWC
conditions.
While
elemental
analysis
and
TGA
is
required
to
establish
the
planned
mass
5
9/
12/
03
of
sample,
the
expected
sample
size
is
on
the
order
of
1
to
2
mg.

The
temperature
in
the
pyroprobe
section
will
be
maintained
at
approximately
50
to
100
o
C
above
the
highest
temperature
for
100%
gasification
across
the
test
materials
as
determined
from
the
thermogravimetric
experiments
earlier
in
the
test
program.
This
is
necessary
to
assure
complete
gasification
of
the
sample
of
test
material
and
a
common
set
of
experimental
conditions
across
the
test
materials
during
combustion
testing.

5.
Combustion
Test
Sampling
and
Analysis
5.1
Exhaust
Gas
Sampling
&
Analysis
Gas
samples
for
off­
line
analysis
will
be
collected
from
a
vent
line
off
the
cold
trap
and
may
be
subjected
to
additional
external
cooling
(
e.
g.,
ice
bath)
as
needed.

Analysis
of
the
exhaust
gas
samples
of
the
thermal
blanks
will
focus
on
PFOA
since
the
primary
purpose
of
conducting
these
blank
runs
is
to
check
for
possible
crosscontamination
between
sample
runs.

5.1.1
Monitored
Parameters
As
noted
in
Section
4.1,
on­
line
monitoring
for
CO
and
CO
2
via
the
in­
line
GC
using
a
molecular
sieve
column
and
MSD
is
planned.
Alternately,
Tedlar
®
bag
samples
of
exhaust
gas
may
be
collected
for
off­
line
CO
and
CO
2
analysis.

Exhaust
gas
flow
rate
will
be
monitored
based
on
measured
input
flow
rates
of
the
synthetic
air
and
methane
gas
feeds.
Exhaust
gas
oxygen
concentration
will
be
calculated,
based
on
measured
input
flow
rate
of
synthetic
air
and
methane
assuming
complete
combustion.

5.1.2.
Fluoride
The
exhaust
gas
will
be
sampled
and
analyzed
for
fluoride
ion
to
assist
in
performing
a
fluoride
balance
across
the
experimental
system.

Fluoride
ion
will
be
sampled
via
absorption
into
aqueous
solution,
using
bubblers
(
low
pressure
drop
midget
6
9/
12/
03
impingers)
in
series.
As
Figure
1
indicates,
initial
plans
call
for
using
three
bubblers
in
series
with
the
first
one
empty
to
serve
as
a
knock­
out
pot
and
the
second
and
third
containing
a
predetermined
amount
of
aqueous
solution.
(
The
number
of
aqueous
solution
bubblers
will
be
adjusted
as
necessary.)
Upon
completion
of
sample
collection,
the
amounts
in
each
bubbler
will
be
measured
and
the
contents
of
the
bubblers
will
be
quantitatively
transferred
into
a
container
for
subsequent
analysis
for
total
inorganic
fluorine
(
i.
e.,
fluoride
ion)
via
ion
chromatography
or
ion
selective
electrode.

5.1.3
Total
Fluorine
The
aqueous
solution
sample
collected
as
described
in
Section
5.1.2
is
also
planned
to
be
subjected
to
analysis
for
total
fluorine
via
Wickbold
torch
so
that
total
organic
fluorine
can
be
determined
by
difference
between
total
fluorine
and
total
inorganic
fluorine.
Work
is
in
progress
to
confirm
that
detection
limits
for
total
fluorine
analysis
via
Wickbold
torch
are
low
enough
to
be
informative
for
this
test
system.

5.1.4
PFOA
Exhaust
gas
samples
will
be
analyzed
for
PFOA
via
LC/
MS/
MS
at
a
qualified
commercial
laboratory
operating
under
suitable
data
quality
guidelines.

Development
is
in
progress
to
define
the
most
suitable
sampling
technique
for
PFOA
in
the
incineration
exhaust
gas.

Initial
plans
call
for
using
the
aqueous
solution
bubblers
described
in
Section
5.1.2
to
collect
PFOA
from
the
exhaust
gas
and
for
sending
a
portion
of
the
aqueous
solution
for
PFOA
analysis
as
described
above.
Additionally,
an
attempt
will
be
made
to
use
an
OSHA
Versatile
Sampler
(
OVS)
as
a
back­
up
sampling
device.
If
OVS
is
also
used
to
sample
PFOA
in
the
exhaust
gas,
then
the
OVS
would
also
be
sent
for
off­
line
LC/
MS/
MS
analysis
to
quantify
PFOA
as
a
crosscheck
on
the
aqueous
solution
bubbler
results.

5.2
Test
Material
Sampling
&
Analysis
Each
test
material
composite
will
undergo
elemental
analysis
for
carbon,
hydrogen,
nitrogen,
fluorine,
sulfur,

7
9/
12/
03
and
oxygen
by
difference.
Ultimate
analysis
(
ASTM
D3176
and
other
ASTM
methods
referenced
therein)
are
planned
for
this
analysis.
Moisture
is
also
determined
by
this
method.
Depending
on
sample
size,
it
may
be
necessary
to
implement
the
microanalytic
analog
of
ultimate
analysis.

Based
on
process
knowledge,
the
level
of
total
fluorine
in
the
test
materials
is
orders
of
magnitude
higher
then
the
potential
level
of
inorganic
fluoride
in
these
materials.
Therefore,
for
this
test
program,
plans
call
for
assuming
that
the
total
organic
fluorine
value
for
each
test
material
composite
is
the
same
as
the
fluorine
value
determined
via
elemental
analysis
as
described
above.

6.
Reporting
of
Results
6.1
Exhaust
Gas
Results
6.1.1
Monitored
Parameters
CO
will
be
reported
in
terms
of
parts
per
million
by
volume
(
ppmv).
CO
2
will
be
reported
in
terms
of
percent
by
volume
(%).
Oxygen
will
be
reported
in
terms
of
percent
by
volume
(%).
Exhaust
gas
flowrate
will
be
reported
in
units
of
cubic
centimeters
per
minute
(
cm
3/
min).

6.1.2
Fluoride
and
Fluorine
Total
fluorine
and
fluoride
(
total
inorganic
fluorine)
in
the
exhaust
gas
will
each
be
reported
in
terms
of
concentration
(
mass
of
fluorine
per
volume
of
exhaust
gas)
in
the
gas
as
well
as
on
the
basis
of
mass
of
fluorine
per
mass
of
starting
test
material.

Total
organic
fluorine
will
be
determined
by
difference
between
total
fluorine
and
total
inorganic
fluorine.

6.1.3
PFOA
PFOA
in
the
exhaust
gas
will
be
reported
in
terms
of
concentration
in
the
gas
as
well
as
on
the
basis
of
mass
per
mass
of
starting
test
material.

8
9/
12/
03
6.2
Test
Material
Results
Elemental
compositions
will
be
reported
in
terms
of
mass
per
mass
of
composite
feed
material.

6.3
Exposure
Assessment
In
the
event
that
PFOA
is
found
in
the
exhaust
gas
at
a
concentration
above
the
limit
of
quantitation
(
for
the
matrix)
from
one
or
more
experiments
described
in
this
protocol,
then
the
potential
for
exposure
related
to
incineration
of
the
subject
material
will
be
assessed
to
inform
the
basis
for
possible
next
steps.

This
assessment
will
consider
a
number
of
factors
such
as
 
Test
program­
determined
PFOA
emission
factor,
 
estimated
amounts
of
subject
material
in
feed
to
fullscale
waste
incinerators,
and
 
degree
of
post­
combustion
air
pollution
control
(
e.
g.,
use
and
effectiveness
of
carbon
adsorption).

9
9/
12/
03
Appendix
Polymers
of
the
sort
being
investigated
in
this
test
program
may
be
present
at
trace
to
low
concentrations
in
municipal
solid
waste
or
in
medical
waste
and
therefore
may
be
incinerated.

A.
1
Types
of
Incinerators
A.
1.1
Municipal
Waste
Combustors
According
to
the
Integrated
Waste
Services
Association
(
IWSA),
there
are
a
total
of
98
waste­
to­
energy
facilities
operating
municipal
waste
combustors
(
MWCs)
in
the
U.
S.
as
of
2002.(
IWSA
2002)
Table
A­
1
summarizes
the
number
and
annual
capacity
of
these
units
by
type
of
technology
employed.

Table
A­
1.
MWCs
in
2002
Type
Number
of
Facilities
Annual
Capacity
(
million
Ton/
year
Mass
Burn
68
22.5
Refused
Derived
Fuel
(
RDF)
18
6.4
Modular
12
0.5
Total
98
29.4
As
the
capacity
values
indicate,
modular
units
are
generally
small
MWCs
accounting
for
less
than
a
total
of
2%
of
the
municipal
solid
waste
incinerated
in
the
U.
S.
in
2002.

A.
1.2
Hospital/
Medical/
Infectious
Waste
Incinerators
Although
earlier
reports
indicated
over
2200
medical
waste
incinerators
in
the
U.
S.
in
the
1990s
(
EPA
2000a),
the
current
EPA
Office
of
Air
Quality,
Planning,
and
Standards
(
OAQPS)
inventory
indicates
that
there
are
116
hospital/
medical/
infectious
waste
incinerators
(
HMIWIs)
in
the
U.
S.
as
of
July
28,
2003.
(
EPA
2003)

This
represents
a
greater
than
90%
reduction
in
the
number
of
operating
HMIWIs
in
the
U.
S.
Many
medical
waste
incinerators
were
closed
rather
than
upgraded
to
meet
new
emission
standards,
as
hospitals
improved
their
programs
to
segregate
infectious
("
red
bag")
waste
burned
in
HMIWIs
10
9/
12/
03
from
non­
infectious
("
black
bag")
waste
handled
as
municipal
solid
waste
after
it
leaves
the
hospital.

A.
2
Operating
Conditions
As
noted
by
EPA,
many
incinerators
for
municipal
solid
waste
are
designed
to
operate
in
the
combustion
zone
at
1800
°
F
[
982
°
C]
to
2000
°
F
[
1093
°
C]
to
ensure
good
combustion.
(
EPA
1995)
EPA
new
source
performance
standards
(
NSPS)
and
emission
guidelines
for
both
municipal
waste
combustors
(
MWCs)
and
hospital/
medical/
infectious
waste
incinerators
(
HMIWIs)
are
based
on
the
use
of
"
good
combustion
practices"
(
GCP).
(
EPA
1997,
EPA
2000b,
EPA
2000c,
Van
Remmen
1998)

Speaking
of
MWCs,
Donnelly
notes,
"
Design
of
modern
efficient
combustors
is
such
that
there
is
adequate
turbulence
in
the
flue
gas
to
ensure
good
mixing,
a
hightemperature
zone
(
greater
than
1000
o
C)
to
complete
burnout,
and
long
enough
residence
time
at
high
temperature
(
1­
2
sec)
for
complete
burnout."
(
Donnelly
2000)
The
term
"
flue
gas"
here
refers
to
the
gas
above
the
grate.

With
respect
to
HMIWIs,
Van
Remmen
states
"
any
unit
which
presently
[
prior
to
compliance
date]
has
a
[
secondary
chamber]
residence
time
less
than
two
seconds
at
1000
o
C
does
not
meet
the
requirement
for
good
combustion
under
the
new
regulations."
(
Van
Remmen
1998)

Similarly,
most
MWCs
are
expected
to
typically
operate
with
a
2
second
gas
residence
time
in
the
high
temperature
zone
in
order
to
assure
compliance
with
emission
standards
on
carbon
monoxide
and
dioxins.

A.
2.1
MWC
Operating
Conditions
EPA
presents
operating
data
for
some
MWCs
in
"
Municipal
Waste
Combustion
Assessment:
Technical
Basis
for
Good
Combustion
Practice"
and
points
the
reader
elsewhere
for
additional
data
on
specific
representative
MWCs.

Modular
MWC
Specifically,
this
background
document
(
EPA
1989)
includes
secondary
chamber
temperatures
for
modular
MWCs
that
had
CO
emission
levels
less
than
current
emission
standards,
and
these
are
summarized
in
Table
A­
2.

11
9/
12/
03
Table
A­
2.
Modular
MWC
Temperatures
Secondary
Chamber
Temperature
(
o
C)
Oswego
Co.,
NY
Red
Wing,
MN
Start
of
campaign
1012
Mid­
range
secondary
temperature
951
End
of
campaign
995
Low
secondary
temperature
885
Mean
secondary
temperature
954
­
1071
As
highlighted
in
Table
A­
2,
typical
secondary
chamber
temperatures
for
these
dual­
chamber
modular
units
are
in
the
range
of
951
to
1071
o
C.

As
indicated
in
section
A.
1,
such
modular
units
are
generally
small
MWCs
and
account
for
less
than
a
total
of
2%
of
the
municipal
solid
waste
incinerated
in
the
U.
S.

Although
this
1989
EPA
background
document
does
not
present
temperature
data
for
mass
burn
nor
RDF
units,
reports
from
the
National
Incinerator
Testing
and
Evaluation
Program
(
NITEP)
present
operating
data
for
an
RDF
combustor
(
Mid­
Connecticut)
and
for
a
mass
burn
waterwall
combustor
(
Quebec
City)
otherwise
discussed
in
the
1989
background
document.

RDF
MWC
Furnace
temperatures
and
flue
gas
oxygen
levels
for
Mid­
Connecticut
RDF
combustor
performance
tests
operating
under
good
combustion
conditions
across
a
range
of
steam
loads
(
Finklestein
and
Klicius
1994)
are
summarized
in
Table
A­
3.

Table
A­
3.
RDF
MWC
 
Mid­
Connecticut
Steam
load
Low
low
Intermediate
Intermediate
normal
normal
normal
high
test
number
PT­
13
PT­
14
PT­
10
PT­
02
PT­
09
PT­
08
PT­
11
PT­
12
Furnace
temperature
(
o
C)
965
1004
1012
1022
1033
1015
1026
1049
flue
gas
O
2
(%)
10.1
9.6
9.2
9.1
7.6
7.5
7.9
6.4
The
average
operating
conditions
for
this
RDF
unit
across
the
range
of
steam
loads
are
1016
o
C
and
8.4%
O
2.

Mass
Burn
MWC
Furnace
temperatures
(
average
of
front
and
rear
radiation
chamber
temperatures)
and
flue
gas
oxygen
levels
(
dry
basis)
for
Quebec
City
mass
burn
combustor
performance
tests
operating
under
good
combustion
conditions
across
a
12
9/
12/
03
range
of
steam
loads
(
Environment
Canada
1988)
are
summarized
in
Table
A­
4.

Table
A­
4.
Mass
Burn
MWC
 
Quebec
City
Steam
load
Low
low
Low
design
design
Design
High
high
test
number
PT02
PT10
PT11
PT05
PT06
PT12
PT07
PT09
Furnace
temperature
(
o
C)
849
875
869
1014
1030
992
1085
1006
flue
gas
O
2
(
dry)
13
13
12
9
9
10
10
10
The
average
operating
conditions
for
this
mass
burn
unit
across
the
range
of
steam
loads
are
965
o
C
and
10.8%
O
2.
When
operated
at
design
steam
load,
the
average
operating
conditions
for
this
mass
burn
MWC
are
1012
o
C
and
9.3%
O
2.

MWC
Summary
Considering
the
relative
quantities
of
municipal
waste
burned
annually
in
each
type
of
MWC
and
the
data
in
this
section,
average
typical
operating
conditions
for
the
high
temperature
zone
of
MWCs
are
nominally
1000
o
C
and
10%
O
2.

A.
2.2
HMIWI
Operating
Conditions
EPA
notes
that
over
97%
of
medical
waste
incinerators
are
controlled
air
modular
units
(
EPA
2000a).
Recent
communication
with
EPA
OAQPS
indicates
that
virtually
all
existing
HMIWIs
are
controlled
air
modular
(
two­
chamber)
units.

Theodore
reports
the
range
of
temperatures
for
the
secondary
chamber
of
controlled
air
medical
waste
incinerators
as
980
to
1200
o
C.
(
Theodore
1990)
EPA
notes
that
auxiliary
fuel
(
e.
g.,
natural
gas)
is
burned
in
the
secondary
chamber
of
medical
waste
incinerators
to
sustain
temperatures
in
the
range
of
985
to
1095
o
C
and
that
combustion
air
at
100
to
300
%
in
excess
of
the
stoichiometric
requirement
is
usually
added
to
the
secondary
chamber.
(
EPA
2000a)

As
noted
above,
a
more
recent
report
indicates
that
existing
HMIWIs
operate
with
secondary
chamber
temperatures
greater
than
or
equal
to
1000
oC
with
a
gas
residence
of
2
seconds.
(
Van
Remmen
1998)

13
9/
12/
03
References
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to­
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