Document ID: EPA-HQ-OPPT-2003-0012-0054
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2003-05-14T04:00Z

TEL~
MEKRESEARC~
H
PROGRAM
AFT
es
February
12,
2003
uring
the
course
of
this
preliminary
study,
the
contract
facility
will
develop
extraction
efficiency
data
on
three
matrices
­
carpet,
textile
and
paper
­
at
three
different
concentrations:
1
ppb,
10
ppb
and
100
ppb
for
articles
only.
In
order
to
do
that
work,
we
have
determined
that
the
contract
lab
needs
individually
prepared
controls
in
the
following
quantity:

Total
pieces:
162
*
I8
of
each
of
these
54
untreated
samples
arc
required/
requested
for
method
development.

Untreated
Articles
Number
of
Samples
Required
for
Analysis
*
Used
to
veri@
extraction
&
iciency
at
1
ppb,
10
ppb
and
100
ppb,
as
well
as
control
WC
plan
on
having
three
different
carpet
samples.

18
samples
analyzed
30
total
treated
and
untreated
articles
I
mber
Treated
Textile
6
Untreated
Textile*
4
2
grams
2
Prams
*
Used
to
veriij
extraction
cfGciency
at
1
ppb,
10
ppb
and
100
ppb,
as
well
as
control
LC/
MS/
MS
Analysis
of
Articles
md
Products
Saqles
and
Suggested
Sampling
Procedure
Marilyn
A.
Stadalius,
Ph.
D.
February
12,
2003
We
plan
on
having
seven
textile
samples.
DRAFT
42
samples
analyzed
70
total
treated
and
untreated
articles
*
Used
to
verify
extraction
efficiency
at
1
ppb,
IO
ppb
and
100
ppb,
as
well
as
control
We
plan
on
having
two
treated
paper
products
analyzed.

I2
samples
analyzed
2.0
total
treated
and
untreated
articles
Number
of
Samples
Required
for
Analysis
Formulation
III
Formulation
IV
40
mL
40
mL
Formulation
V
Formulation
VI
1
40
mL
1
40
mL
Formulation
VII
Formulation
VIII
Formulation
IX
Formulation
X
Formulation
XI
1
40
mL
I
1
1
/
Formulation
XII
1
40
mL
2
LC/
MS/
MS
Analysis
of
Articles
and
Products
Samples
and
Suggested
Sampling
Procedure
Marilyn
A.
Stndalius,
Ph.
D.
February
12,
2003
DRAFT
This
study
should
be
viewed
as
a
screening
study.
Currently,
a
validated
methodology
does
not
exist
for
the
analysis
of
the
test
substance
in
carpet
(
shavings),
textiles
and
paper.
The
purpose
of
the
preliminary
study
is
to
demonstrate
the
suitability
of
the
existing
LC!
MS,/
MS
method
to
analyze
the
test
substance
in
your
matrices.
A
report
detailing
the
methodology
used
to
obtain
70­
l
10%
extraction
efficiencies
for
1
ppb,
10
ppb
and
100
ppb
test
substance
in
each
of
these
three
matrices
will
be
available
to
all
TRP
members.
The
accuracy
and
precision
of
the
method­
ology
will
be
determined
by
extracting
6
untreated
articles
(
each
of
carpet,
paper
and
textile)
each
at
1
ppb,
10
ppb
and
100
ppb
on
two
successive
days.

Once
validated
and
verified
for
accuracy
and
precision,
this
method
will
be
used
to
analyze
our
now
12
treated
articles.
In
order
to
minimize
the
variability
in
sampling,
it
is
key
that
steps
be
taken
to
generate
a
representative
sample
for
each
treated
article.
It
is
important
that
the
sampling
procedures
used
to
generate
these
samples
be
documented
and
retained
in
your
study
records.

A.
Textile
Sampling
Procedure
etermine
the
size
of
a
2­
gram
sample
of
paper.

2.
Suggested
sampling
approach:

Treated
Samples
from
Roll
of
Fabric
­
If
the
treated
sample
is
taken
from
a
roll,
first
discard
a
minimum
of
1
meter
of
fabric
from
the
very
outside
of
the
roll
­
equivalent
to
at
least
one
wrap
­
then
take
a
full­
width
swatch
0.5
meter
long
from
the
end
of
the
roll
of
fabric.

­
Create
a
grid
with
pencil
on
the
treated
fabric,
eliminating
3­
5
cm
from
the
fabric
edges.
The
grid
should
be
composed
of
six
equivalent
blocks.
These
six
blocks
represent
the
six
areas
where
you
will
take
one
sample.
Divide
each
of
the
large
blocks
into
smaller
blocks,
so
that
each
sub­
block
is
equivalent
to
a
2­
gram
sample.
Systematically
number
all
the
smaller
blocks
in
each
larger
block.
Use
a
random
number
generator
(
in
Excel)
to
generate
a
list
of
random
numbers
between
1
and
the
number
of
smaller
blocks
in
each
larger
block.
Use
the
first
six
numbers
to
select
the
six
locations
of
the
treated
article
sample
in
each
larger
block.

Treated
Samples
from
Discrete
Squares
of
Fabric
­
If
each
discrete
square
of
treated
fabric
is
small
enough
to
generate
one
to
six
samples,
take
one
random
sample
from
each
discrete
square
of
treated
fabric
using
the
block
design
concept
described
above.
Therefore,
from
six
discrete
squares
of
treated
fabric,
take
one
random
sample.

Untreated
Fabric
Samples
Untreated
fabric
samples
can
be
taken
randomly
from
untreated
fabric
­
avoid
edges
­
avoid
contamination;
supply
four
untreated
samples.
LC;`
MS/
MS
Analysis
of
Articles
and
Products
Samples
and
Suggested
Sampling
Procedure
Marilyn
A.
Stadalius,
Ph.
D.
F&
wary
12,
2003
DRAFT
ocumcnt
the
sampling
approach.

etermine
the
size
of
a
2­
gram
sample
of
paper.

2.
Suggested
sampling
approach:

Treated
Samples
from
Roll
of
Paner
­
If
treated
sample
is
taken
from
a
roll,
first
discard
a
minimum
of
1
meter
of
paper
from
the
very
outside
of
the
roll
­
equivalent
to
at
least
one
wrap
­
then
take
a
full­
width
swatch
0.5
meter
long
from
the
end
of
the
roll
of
paper
in
the
lot
sample.

­
Create
a
grid
with
pencil
on
the
paper,
eliminating
3­
5
cm
from
the
paper
edges.
The
grid
should
be
composed
of
six
equivalent
blocks.
These
six
blocks
represent
the
six
areas
where
you
will
take
one
sample.
Divide
each
of
the
large
blocks
into
smaller
blocks,
so
that
each
sub­
block
is
equivalent
to
a
2­
gram
sample.
Systematically
number
all
the
smaller
blocks
in
each
larger
block.
Use
a
random
number
generator
(
in
excel)
to
generate
a
list
of
random
numbers
between
I
and
the
number
of
smaller
blocks
in
each
larger
block.
Use
the
first
six
numbers
to
select
the
six
locations
of
the
treated
article
sample
in
each
larger
block.

Treated
Samples
from
Discrete
Squares
of
Paper
­
If
each
square
of
discrete
treated
paper
is
small
enough
to
generate
one
to
six
samples,
take
one
random
sample
from
each
square
of
treated
paper
using
the
block
design
concept
described
above.
Therefore,
from
six
discrete
squares
of
treated
paper,
take
one
random
sample.
Collect
six
samples.

Untreated
Paper
Samples
­
Untreated
samples
can
be
taken
randomly
from
untreated
paper
­
avoid
edges
­
avoid
contamination;
supply
four
untreated
samples.

ocument
your
sampling
approach.

C.
Carnet
Sampling
Procedure
1.
Determine
the
size
of
carpet
that
will
produce
approximately
1
O­
grams
of
carpet
shavings.

2.
Suggested
sampling
approach:

Samples
from
Discrete
Sections
of
Car­
net
­
If
each
discrete
section/
square
of
treated
carpet
can
generate
one
to
six
samples,
take
one
random
sample
from
each
section
of
treated
carpet
using
the
block
design
concept
described
above
for
textile
and
paper.
Therefore,
from
six
discrete
squares
of
treated
carpet
take
one
random
sample.

4
LC/
MS/
MS
Analysis
of
Articles
and
Products
Samples
and
Suggested
Sampling
Procedure
Marilyn
A.
Stadalius,
Ph.
D.
February
12,
2003
DRAFT
­
When
sample
location
is
identified,
use
hair
shears
to
remove
carpet
shavings
(
fibers)
from
the
carpet
backing.
Shear
fibers
as
close
to
carpet
backing
as
possible.
It
is
recommended
to
clear
the
hair
shears
with
cheesecloth,
as
cheesecloth
should
not
be
contaminated
with
the
test
substance.

Untreated
Samples
of
Carpet
Untreated
samples
of
carpet
can
be
taken
randomly
from
untreated
carpet
­
avoid
edges
­
avoid
contamination;
supply
four
untreated
samples
of
carpet
shavings.

ocument
your
sampling
approach.

A.
Articles
­
Triple
wrap
each
sample
with
aluminum
foil.
For
a
IO­
cm
square
sample,
cut
a
piece
of
foil
that
is
at
least
25­
cm
long.
Fold
foil
at
the
mid­
point
of
the
length.
Place
article
in
the
pocket.
Fold­
up
about
1
cm
on
each
edge.
Fold
up
another
cm
of
each
edge.
Then
crimp
tight.
Repeat
with
two
more
pieces
of
aluminum
foil.
Place
in
zip­
lock
bag
­
remove
air
from
bag
and
seal.

­
Place
in
a
second
zip­
lock
bag.
Place
provided
labels
with
sample
identification
numbers
on
outside
of
second
plastic
bag.
Sample
should
be
labeled
with
Project
Number,
Sample
Identification
Number
and
sample
type.
Sample
label
should
also
clearly
state
if
sample
is
treated
or
untreated.
Complete
Sample
Identification
Sheet
for
the
study
records.

­
Sample
identification
numbers
have
been
provided
in
excel
spreadsheet.
Labels
will
be
shipped
on
February
13,2003.

­
Pack
untreated
sample
separately
from
treated
samples
­
Include
a
chain­
of­
custody
form
in
each
package.

­
Follow
shipping
procedure.

.
Products
­
Place
40
mL
of
product
formulation
used
to
treat
article
in
the
appropriate
containers
for
shipment.
Double­
bag
each
sample,
using
zip­
lock
plastic
bags.
Place
label
with
sample
identification
number,
project
number
and
sample
lot
number
on
outside
of
second
plastic
bag.
Include
chain­
of­
custody
form
and
modified
MSDS
in
box
containing
formulated
product
samples.
Ship
products
separately
from
articles.
Follow
shipment
procedures.
Complete
Sample
Identification
Sheet
for
the
study
records.