Document ID: EPA-HQ-OPPT-2003-0012-0053
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2003-05-14T04:00Z

Telomer
Research
Program
Analysis
of
Telomer­
Based
Products
and
Telomer­
Treated
Articles
Scope
and
Rationale
The
Telomer
Research
Program
(
TRP)
1
has
studies
underway
to
investigate
the
potential
formation
and/
or
release
of
perfluorooctanoic
acid
(
PFOA)
from
telomer­
based
products
and
consumer
articles
treated
with
such
products.
The
purpose
of
this
work
is
to
determine
whether
articles
treated
with
representative
telomer­
based
products
contribute
to
significant
human
or
environmental
exposure
to
PFOA.
The
full
scope
of
the
program
is
outlined
in
the
TRP
Letter
of
Intent.
2
Project
Overview
The
TRP
has
contracted
with
an
outside
research
laboratory
to
analyze
for
the
presence
of
PFOA
in
the
major
telomer­
based
products
in
commerce
and
articles
treated
with
those
products.
This
screening
study
will
investigate
levels
of
PFOA
in
the
three
major
end­
use
categories:
carpets,
textiles
and
paper.
The
primary
products
that
the
TRP
members
market
for
these
applications
are
polymers,
which
represent
approximately
85%
of
the
telomer­
based
products
that
the
TRP
members
manufacture
and
sell.
The
product
classes
to
be
tested
are
those
that
the
respective
TRP
member
companies
manufacture
as
actual
items
of
commerce.

While
there
are
many
potential
telomer­
based
polymeric
products,
a
relatively
small
number
represent
the
primary
product
classes
in
commerce
(
12
products).
The
results
of
this
screening
study
will
provide
a
comprehensive
initial
picture
of
exposure
potential
by
focusing
on
these
major
end­
use
polymeric
products
and
the
corresponding
articles
of
commerce.
The
treated
articles
to
be
tested
are
actual
carpet,
textile,
and
paper
substrates
treated
under
representative
or
actual
mill
conditions
with
the
subject
telomer­
based
polymeric
products.

Approach
and
Methodology
Method
Development
and
Validation
A
significant
amount
of
work
was
required
to
develop
and
coordinate
the
appropriate
sampling,
shipment
and
analysis
plans
as
well
as
to
synthesize
and
characterize
primary
and
[
1,2­
13
C]
perfluorooctanoic
acid
analytical
standards.
This
initial
work
was
conducted
by
analytical
experts
from
the
TRP
member
companies
in
parallel
with
efforts
to
solicit
bids
from
potential
contract
labs.
The
initial
work
by
the
contract
lab
will
require
method
development
for
quantita­
tive
determination
of
PFOA
in
the
various
article
matrices
and
telomer­
based
products
as
well
as
1
The
companies
participating
in
the
TRP
include
Asahi
Glass,
Clariant
GmbH,
Daikin
Industries
and
E.
I.
duPont
de
Nemours
&
Company.
2
Letter
of
Intent
for
the
Telomer
Research
Program
submitted
to
Stephen
L.
Johnson
(
US
EPA)
on
March
14,
2003.
Ref.
AR226­_______.

Does
not
contain
TSCA
CBI
TRP
(
31­
Mar­
03)
1
validation
of
the
methodology
for
determining
PFOA
in
treated
articles.
More
on
method
development
and
method
validation
is
discussed
below.

Article
Analysis
Samples
of
the
12
telomer­
treated
articles
will
be
collected
from
pilot
plant
facilities
or
from
commercial
manufacturing
facilities
and
analyzed
for
PFOA
using
the
developed
and
validated
analytical
method.
The
study
is
designed
as
a
screening
study
to
determine
whether
PFOA
is
present
in
each
treated
article
collected,
and
if
it
is
present,
at
what
levels
and
the
confidence
of
those
reported
levels.

Types
of
Articles:
representative
textile,
carpet
and
paper
articles
(
12
total)

An
LC/
MS/
MS
methodology
using
a
[
1,2­
13
C]
perfluorooctanoic
acid
internal
standard
will
be
used
for
these
analyses
having
the
objective
of
attaining
a
lower
limit
of
quantification
of
1
part
per
billion
(
ppb)
with
a
relative
standard
deviation
of
less
than
20%.

Method
development
will
be
conducted
with
the
goal
of
having
extraction
efficiencies
fall
within
70­
110%
for
three
matrices
­­
carpet
(
nylon),
textile
(
polyester)
and
paper
­­
at
the
three
PFOA
fortification
levels
of
1
ppb,
10
ppb
and
100
ppb.

One
hundred
sixty
two
(
162)
untreated
shaved­
carpet,
textile
and
paper
samples
were
generated
for
the
method
development
and
method
validation
portion
of
this
study.
If
scouting
experi­
ments
show
acceptable
recoveries
at
the
levels
noted,
the
contract
lab
will
proceed
with
method
validation.

Method
Validation
for
PFOA
in
Articles:
The
method
for
the
determination
of
PFOA
in
treated
articles
will
be
validated
at
1
ppb,
10
ppb
and
100
ppb
in
each
of
carpet
(
nylon),
paper
(
cellulose)
and
fabric
(
polyester)
under
Good
Laboratory
Practices
(
GLP).
Method
validation
will
comprise
of
demonstrating
the
accuracy
and
precision
of
the
method
by
analyzing
six
samples
spiked
at
each
fortification
level
on
two
separate
days.
Hence,
36
samples
for
each
article
­­
6
each
at
1
ppb,
10
ppb
and
100
ppb
on
each
day
­­
will
be
analyzed
for
a
total
of
108
analyses
over
the
two­
day
period
of
the
method
validation.
Analysis
of
articles
will
not
proceed
until
method
validation
and
protocol
for
analysis
of
articles
has
been
approved.

Samples:
Each
of
the
12
articles
tested
will
be
treated
with
a
single
telomer­
based
polymeric
product.
Six
(
6)
sub­
samples
will
be
analyzed
for
each
article/
product
pair,
selected
using
a
block
design
approach.
Seventy­
two
(
72)
sub­
samples
for
articles
(
12
treated
articles
x
6
sub­
samples)
will
be
generated
and
twelve
(
12)
products
will
be
collected
for
analysis
resulting
in
four
unique
carpet/
product
pairs,
six
unique
textile/
product
pairs
and
two
unique
paper/
product
pairs.
Included
for
each
of
the
12
articles
will
be
4
untreated
samples
to
be
used
as
control
and
for
extraction
efficiency
verification.

Product
Analysis
This
screening
study
is
designed
to
determine
the
level
of
PFOA
in
each
product
class
using
an
LC/
MS/
MS
method.
Matrix
complexities
may
make
these
analyses
particularly
challenging.

Product
Types:
acrylate
and
urethane
polymers
(
12
product
formulations)

Does
not
contain
TSCA
CBI
TRP
(
31­
Mar­
03)
2
Samples
of
the
12
primary
telomer­
based
polymeric
products
will
be
provided
by
TRP
member
companies
to
the
contract
lab
for
analysis.
A
standard
addition
approach
using
LC/
MS/
MS
methodology
is
being
used
for
these
analyses
of
telomer­
based
products,
having
lower
limit
of
quantification
for
PFOA
of
1
part
per
million
(
ppm)
with
a
relative
standard
deviation
of
20%.
A
[
1,2­
13
C]
perfluorooctanoic
acid
internal
standard
will
be
used
throughout
the
study.
Before
the
product
samples
are
analyzed,
extraction
efficiencies
will
be
evaluated
on
at
least
two
or
three
product
groups
using
modified
methodologies
supplied
by
the
TRP.
Product
analyses
are
being
conducted
under
GLP.

Results
The
results
of
this
screening
study
will
be
prepared
as
a
report,
including
the
following
details:

Summary
of
Method
and
Results
Materials
used
Equipment
used
Reagents
and
standards
used
Analytical
Procedures
Preparation
of
stock
standard
solution,
preparation
of
fortification
of
articles
and
preparation
of
calibration
standards
Pre­
processing
of
samples,
sample
fortification
procedures,
analyte
extraction
and
final
sample
preparation
procedures
Instrumentation
LC/
MS
conditions
LC/
MS
Calibration
and
Samples
Analysis
Calculation
Methods
Results
and
Discussion
Detector
response
Control
and/
or
Blank
Recoveries
Extraction
Efficiency
Limit
of
Quantification
and
Limit
of
Detection
Conclusions
Schedule
Work
by
the
TRP
analytical
experts
began
in
January
2003
to
develop
the
appropriate
sampling,
shipment
and
analysis
procedures
as
well
as
primary
and
[
1,2­
13
C]
perfluorooctanoic
acid
analytical
standards
for
the
proposed
work.
In
concert
with
this
effort,
potential
contract
labs
were
identified
and
bids
were
solicited.
The
selected
laboratory
received
the
final
study
plans
and
sample
requirements
in
February
2003.
The
internal
standard
was
prepared
by
one
of
the
TRP
companies
and
delivered
to
the
lab
in
March
2003.

Does
not
contain
TSCA
CBI
TRP
(
31­
Mar­
03)
3
Does
not
contain
TSCA
CBI
TRP
(
31­
Mar­
03)
4
The
initial
work
to
develop
and
validate
analytical
and
sample
methods
will
be
conducted
in
March 
April
2003.
The
analysis
of
telomer­
treated
articles
and
telomer­
based
polymeric
products
will
be
initiated
in
April
2003.
The
final
report
is
expected
by
June
/
July
2003.
The
results
will
be
provided
to
EPA
as
soon
as
they
become
available.