Document ID: EPA-HQ-OPPT-2002-0056-0041
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2002-09-17T04:00Z

*

­­
­f
DOW
USA
Texas
Operations
The
Dow
Chemical
Company
2301
Brazosport
Blvd
Freeport,
Texas
77541­
3257
July
27,200l
WIL
Research
Laboratories,
Inc.
ATTN:
Peter
Voytek
1407
George
Road
Ashland,
OH
44805­
928
1
RE:,
Analysis
of
1,1,2­
Trichloroethane
samples
Dear
Mr.
Voytek:

I
received
two
samples
of
1,
I
,2­
trichloroethane
from
you
on
the
afternoon
of
7/
25/
O
1.
Reference
numbers
for
the
samples
are:
WIL­
4
1700
1
and
WIL­
4
17002.
The
samples
were
returned
for
assay
or
determination
of
the
purity
of
the
1,1,2­
trichloroethane.
The
samples
were
analyzed
that
same
afternoon
in
our
Quality
Assurance
lab
which
does
the
analytical
work
for
the
release
of
our
product.
The
results
are
as
.foliows:

WIL­
4
1700
I
WIL
417002
1,
I
,2­
trichloroethane
99.546
Wt
%
99.549
Wt
%
1
,l
,
1
,ZTetrachloroethane
0.0600
Wt
%
0.0588
Wt
%
normal
process
impurity
1,2­
Butylene
Oxide
.
0.1893
Wt
%
0.1895
Wt
%
stabilizer
Secondary
Butanol
0.2047
Wt
%
0.2023
Wt
%
stabilizer
This
material
is
Stabilized
1,1,2­
Trichloroethane.
The
1,2­
butylene
oxide
serves
as
an
acid
acceptor
and
provides
stability
against
metals.
The
secondary
butanol
serves
to
provide
stability
against
metals.
.

The
analysis
was
done
by
gas
chromatography.
The
method
is
as
follows:
.

Column
)
DB
1701
1
u
film
thickness,
0.32
mm
X
60
meter
Temperature
program
1
Initial
Temp
of
40°
C
for
3
min
I
1
10"
Cimin
to
200°
C
I
Carrier
gas
Split
ratio
stop
Helium
at
a
constant
flow
of
3
cc/
min
200:
1
.

.
As
you
know,
Dow
is
a
producer
of
1,1,2­
trichloroethane
and
producer
of
the
material
being
analyzed
I
,
believe.
We
routinely
analyze
this
material.
We
calibrate
the
gas
chromatographs
with
standards
containing
the
known
process
impurities
and
stabilizers
in
concentrations
in
the
range
that
these
impurities
and
standards
are
normally
present.
We
prepare
the
standards
from
pure
components
using
an
analytical
balance.
We
determine
the
concentration
of
impurities
and
stabilizers
present
and
then
determine
assay
of
the
1,1,2­
trichloroethane
by
subtracting
the
sum
of
the
impurities
and
stabilizers
from
100%.
It
is
probably
quite
obvious
that
this
method
gives
greater
precision
than
does
measuring
the
concentration
of
the
1,1,2­
trichloroethane
directly.
The
following
simple
example
illustrates
this.
Let
us
assume
that
the
relative
standard
deviation
of
the
gas
chromatographic
analysis
is
13%.
It
is
certainly
obvious
then
that
the
results
of
direct
measurement
of
the
component
that
is
almost
100%
of
the
total
will
have
a
standard
deviation
of
about
3%.

j
2
Now
let
us
assume
that
same
3%
RSD
applies
to
each
of
the
three
measured
components
then
the
combined
relative
standard
deviation
for
the
three
components
is:
.

.

l
l
.

I
RSD,
=
,/­=
5.2%

5.2%
of
a
total
of
about
0.45
wt
%
stabilizer
plus
impurity
is
about
kO.
O23%
compared
to
*3%
for
direct
measurement.

I
am
enclosing
copies
of
the
GC
scans.
Note
the
following
internal
GC
scans
and
computer
prints
outs.
slang
term
and
short
cuts
as
on
the
BO
z
1,2­
Butylene
Oxide
SBA
=Z
Secondary
Butanol
1112,
tetra
=
1
,
1,1,2­
tetrachloroethane
B­
Tri
(Beta­
Tri
or
p­
Tri)
=
1
I
1,2­
trichloroethane
Acetone
is
not
a
process
impurity
but
a
rinse
solvent
between
sample
vials
on
the
autoinjector.
Most
of
the
small
area
counts
seen
on
the
computer
printout
is
baseline
noise
as
can
be
seen
by
comparing
it
to
the
scan.
The
product
can
also
contain
trace
amounts
(co.
01
wt
%)
of
ethylene
dichloride,
trichloroethylene
and
bromochloroethane,

If
I
can
be
of
further
assistance
please
do
not
hesitate
to
contact
me.
,

Regards,

Chlorinated
Organic
Products
Technologies
Center
Building
A­
2422
Office:
979­
238­
4232
Pager:
888­
437­
679
1
FAX:
979­
238­
0136
E­
Mail
dougterry@
dow.
com
.
.
.

July
24,2001
Mr.
Douglas
Terry
The
Dow
Chemical
Company
2301
N.
Brazosport
Blvd.
Building
A­
2422
Freeport,
TX
77541
Ref:
WIL­
4
17001
and
.
.
WL4!
7002
Dear
Mr.
Terry:

Enclosed
please
find
two
samples
of
1,
I,
2­
Trichloroethane
that
were
collected
on
July
.
20,
2001
from
the
bulk
test
article
containers
used
for
the
above­
referenced
studies.
The
­
test
article
and
samples
have
been
stored
under
ambient
conditions.

For
our
records,
please
acknowledge
receipt
of
these
samples'and
paperwork
by
signing
the
statement
below
and
returning
either
the
original
or
a
copy
of
this
letter
to
me.
.
.

If
you
have
any
questions,
please
call
me
at
(419)
289­
8700.
.

c
c
Sincerely,

I
.

GRIUsrs
&@
Manager,
Inhalati&
Toxicology
.:
*CC:
Peter
Voytek
.

Enclosures
I,
the
undersigned,
ackn
above­
referenced
samples
and
paperwork.

W&,`
RESEARCH
LABO~
ATORIES.~
XC
1407CEO~
GERO,
4D
ASHLAND.
OH
!4805­
9281
(qlg)
2898700
FM(
41CjQ89­
3650
,
.
improving
human
health
and
protecting
the~
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throuih
scientific
research
services.@
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1
SOLVENTS
SAMPLE
WORKSHEET1
_____­____­­­____­__­­­­­­­­­­­­­­­­­­­­­­­­­­­­

3
Worksheet
prepared
on
25­
JUL­
2001.
Ir.

Sample
ID
:
56260
Text
ID
:
B­
TRI­
S­
JUL­
25­
52
.
Comments
:
#5015A
#1
PRODUCT
:
B
TRI
S
SPEC
LEVEL
:
PRODUCTION
LOT
NUMBER
:
SAMPLE
TYPE
:
TEST
LOGIN
DATE
:
25­
JUL­
2001'18:
36
SHIPMENT
:
CARRIER
ID
:
COMPARTMENT
:
LOGIN
BY
:
u137519
­­­­­­­­­­­­­­­­­­­­­­­­­=
==========================================­­­­­­­­­­­­­­­­­­­

The
following
tests
have
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assigned
to
this
sample:
­_­­­­__­­­­­­­
__­­­­­­­­­­­­­­____­­­­­­­­­­­­­­­­­­­

­__________­___­___­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­.

I
Analysis
I
Component
Name
1
MIN
I
MAX
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Result
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Chemical
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56260.
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1
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_____­_­­__­_­­­­­­­­­­­­
­­­____________________

1
SOLVENTS
SAMPLE
WORKSHEET/
_______­___­_____­__­­­­­­­
­­_____________
­we_­­

Worksheet
prepared
on
25­
JUL­
2001.

Sample
ID
:
56260
Text
ID
:
B­
TRI­
S­
JUL­
25­
52
Comments
:
#5015A
#l
­w­
s­­­
____­__­­­_­­­­
­­_­­_____________
_­­­­­_­­­­­

PRODUCT
:
B
TRI­
S
SPEd
LEVEL
:
PRODUCTION
LOT
NUMBER
:
SAMPLE
TYPE
:
TEST
LOGIN
DATE
:
25­
JUL­
2001
18:
36
.
SHIPMENT
:
CARRIER
ID
:
COMPARTMENT
:
LOGIN
BY
:
U137518
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­­­­­­­=­­­
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­­­­­­­­­­­­­======­­­­=========­­­­=======­
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The
following
tests
have
been
assigned
to
this
sample:
­___________­_­_­___­­­­­­­­­­­­
­_____________
w­­­­­
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%­"

_­___­__­_­­­­­­­­­­­
­­­__­_­­~­­­­­­­­­
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­­______­­_­­­­­

Analysis
1
Component
Name
I
MIN
I
MAX
I
Result
I
Units
­­­__­
m­
m­
_­+­­­­­­­­­­­­­­­­­­­­­­­+­­­­­­­­+­­­­­­­~­­­­­­­­­­­­
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ASSAY­
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1
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lo.
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1
3
04'3
I
%wt
.
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+­­­;­­­­­­­­­­­­­+­­­­­­­
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1
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Tetra
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*I
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%wt
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The
Dow
Chemical
Company
.
Dow
Confidential
L
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[TERMItiALk­
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l
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Reported
on
25­
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2001
at
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06
.
Page
1
Injection
Report
Acquired
on
25­
JUL­
2001
at
18:
48
TXVG02
Texas
Division
Manufacturing
Labs
.

Analyst
Name
:
REED
Lims
Id
:
ASSAY­
BTRI
Comment
:
#SO15
#l
Method
Title
:
B­
Tri
(1,1,2­
Trichloroethane)
Sample
Name
:
B­
Tri
(1,1,2­
Trichloroethape)
Sample
Id
:
56260
Sample
Type
:
Sample
Amount=
l.
OOOOO
Bottle
No
:
1
PEAK
INFORMATION
Peak
RT
mins
RT
Val
Area
uVs
wt
%
Peak
name
RF
slope
RF
intercept
­

1
2.120
0.000
2
2.169
0.000
3
2.307
0.000
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3.293
0.000
3.751
0.000
,­
6
4.062
0.000
7
4.276
0.000
a
4.336
0.000
9
5.222
0.000
10
5.533
0.000
11
7.360
0.000
12
8.453
0.000
13
9.643
0.000
14
9.809
0.000
15
10.462
0.000
16
11.413
0.000
17
12.107
0.000
18
12.280
0.000
19
12.658
:o.
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20
13.058
0
:ooo
21
15.133
0.000
22
15.502
0.000
23
15.911
0.000
24
16.244
0.000
25
16.693
0.000
26
16.933
0.000
1439
0.0000
1155
0.0000
619
0.0000
a12
0.0000
3408880
0.1893
2024
0.0000
2286
0.0000
3202291
0.2047
3864
0.0000
4968
0.0000
676d2
0.0000
23419694
99.5460
313447
0.0600
2452
0.0000
3027
0.0000
1341
0.0000
10079
0.0000
994
0.0000
1070
0.0000
1946
0.0000
535
0.0000
a10
0.0000
1452
0.0000
1887
0.0000
505
0.0000
a78
0.0000
Totals
Unknowns
111802
0.0000
30344312
100.0000
30456114
100.0000
c
`.

L
.
0.0000
0.0000
0.0000
.
0.0000
BO
17924366.0000
­
0.0000
0.0000
SBA
15575979.0000
c
0.0000
0.0000
0.0000
B­
Tri
234207.0469
1112,
Tetra
5202291.5000
0.0000
0.0000
0.0000
­
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
.
.

.

"
/

0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0
.
0.0
0
0
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
l
.

Intanslty
(rnV1
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.
.
.

l
L
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Sample
Wo.
rksheet
:
56261
Page
1
m
.
:­­
.
.
______­­­­­­­­­­­
'­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­
1
SOLVENTS
SAMPLE
WORKSHEET1
______­­­­­­­­­­_­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­

Worksheet
prepared
on
25­
JUL­
2001.

Sample
ID
:
56261
Text
ID
:
B­
TRI­
S­
JUL­
25­
53
Comments
:
#5015A
#2
__________­­­­­­__­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­

PRODUCT
:
B
TRI
S
SPEC
LEVEL
:
PRODUCTION
LOT
NUMBER
:
SAMPLE
TYPE
:
TEST
LOGIN
DATE
:
25­
JUL­
2001
18:
38
SHIPMENT
:
CARRIER
ID
:
COMPARTMENT
:
LOGIN
BY
:
u137519
______­_­­­­­
­=====================================­­­­­­­­­­­­­­­­­
­­_­­_­­­­­­­­

The
following
tests
have
been
assigned
to
this
sample:
_­_____­___­­­­­­­­­­­­
­­­­__________________________

~­­_­__­­___­­­­__­_~­­
­­­­­_______________­­­­­­­­­­­­­­­
__
____
­­­­­­

I
Analysis
1
Component
Name
1
MIN
I
MAX
I
Result
I
Units
;
I
­­­­­­­
­­­­­+­­­­­­­­­­­­­­­­­­­­+­­­­+­­­
­­­­­
+­­­­­­­+
­­­­­­­­­­­­­­­­+­­­­­­­
I
I
ASSAY
BTRI/
I
BO
10.100
10.200
10.1895
%wt
I­­­­­
­­­­­­­+­­­­­­­­­­­­­­­­­­­­­­­+­­­­­­­­+­­­­­­­+­­­­­­­­­­­­­­­­+­­­­­­­

I
1
SBA
10.200
10.350
10.2023
%wt
I
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l
c
`.

$
The
Dow
Chemical
Company
c
.
Dow
Confidential
.
.
s­.
_
­

L
c
u
sample:­
yorksheet
:
562681
l
l
Page
____­­­­­­­­
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­­­­m
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­­­­

1
SOLVENTS
SAMPLE
WOR.
KSHEETI
,
___­­­­­­­­­­­­__­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­

Worksheet
prepared
on
25­
JUL­
2001.

Sample
.ID
:
56261
Comments
:
#5015A
#2
Text
ID
:
B­
TRI­
S­
m­
25­
53
______­­­­­­­­­­­­­­­
­­­­­­­­­­­­­­­_____­­­­­­­­­­­

PRODUCT
:
B
TRI
S
SPEC
LEVEL
:
PRODUz;
TION
SHIPMENT
:
LOT
NUMBER
:
CARRIER
ID
:
SAMPLE
TYPE
:
TEST
COMPARTMENT
:
LOGIN
DATE
:
25­
JUL­
2001
18:
38
LOGIN
BY
:
u137519
1
.

The
following
tests
have
been
assigned
to
this
sample:
t
c
________________­_­­­­­­­­­­­­­­­
­­­­­­­_____________

____­­­­­­­­
_____­­­­­­­^­­­­­­­­­
­­­­­­­­­___________­­­­­­­­­­­­­­­­­­­­­­­­

Analysis
1
Component
Name
I
MIN
I
­
I
Res;
lt
1
Units
­­­­­­
e­
v­­­+­­
_­­­­­­­­­­­­­­­­
­­­­+­­­­­­­­+­­­­­­­+­­­­­­­­­­­­­­­­+­­­
­­­­
ASSAY­
BTRI/
lj
BO
I
0.100
10.20b
1
­­­­­­­
w­­
m­+­­
­­­­­­­­­­­­­­­­­­­­­
f­­
lW2
­­­­
yw'­­
­­­­­­+­­­­­­­+­­­
J­­
­­­
­­

­,.
1
SBA
%wt
.

j
10.200
10.350
1
­­­­­
e­­
s+­­­­
­­­­­­­­­­­­­­­­­­­+­­­­­­­­+­
b
203­
3
`_____­_
­­­­­­+­­­­­­­­­­­­­­­­+

­5
1
1112,
Tetra
I
I
l
I
I
%wt
­­­­­­
O~~~­­­­­+­­­­.
­­­­­­+­­­­­­­­­­­­­­­­­­­­­­­+­­­­­­­­+­­­­­­­+­­­­­~­­­
I
B­
Tri
I
I
I
­­­­­­­­­­­­+­­­­­­­­­­­­­­­
`­­­­­­­+­­­­­­­­
t­­­­­­­+­­­­­­­­­­­­

.

The
D,
ow
Chemical
Company
Dow
Confidential
.
.
.

L
I
I
.[
TERMINA+
l91
BTR25JUL011919,?.,
1
,
.
Page
1
Reported
on
25­
JUL­
2001
at
19:
41
­3
"L
Injection
Report
Acquired
on
25­
JUL­
2001
at
19:
22
TXVG02
Texas
Division
Manufacturing
Labs
Analyst
Name
:
.ED
Lims
Id
:
ASSAY­
BTRI
Comment
:
#5015A
#2
Method
Title
:
B­
Tri
(1,1,2­
Trichloroethane)
Sample
Name
:
B­
Tri
(1,1,2­
Trichloroethane)
Sample
Id
:
56261
Sample
Type
:
Sample
Amount=
l.
OOOOO
Bottle
No
:l
.

PEAK
INFORMATION
Peak
RT
mins
RT
Val
Area
uVS
wt
%
Peak
name
RF
slope
RF
interce0t
1
2.120
0.000
2
2.164
0.000
3
2.307
0.000
2.529
3
0.000
­­­
3.013
0.000
6
3.747
0.000
7
4.084
0.000
8
4.289
0.000
9
4.396
0.000
10
5.240
0.000
11
5.547
0.000
12
7.360
0.000
13
8.578
0.000
14
9.644
0.000
15
9.840
0.000
16
10.489
0.000
17
11.427
0.000
18
12.111
0.000
19
12.280
:o.
ooo
20
12.662
o.\
ooo
21
13.062
0.000
22
14.809
0
..
ooo
23
15.173
0.000
24
15.853
0.000
25
16.800
0.000
26
16.929
0.000
27
17.151
0.000
28
17.316
0.000
29
17.556
0.000
i`
17.809
I
0.000
­r'
1429
0.0000
1132
0.0000
562
0.0000
6722
0.0000
16646
0.0000
3403460
0.1895
951
0.0000
1249
0.0000
3157367
0.2023
3965
0.0000
4763
0.0000
67020
0.0000
23356414
99.5494
306209
0.0588
4906
0.0000
2572
0.0000
1262
0.0000
8952
0.0000
894
0.0000
1238
0.0000
1824
0.0000'

746
0.0000
940
0.0000
1001
0.0000
512
0.0000
3991
0.0000
4502
0.0000
862
0.0000
1022
0.0000
4595
0.0000
'
0.0000
0.0000
0.0000
.

Acetone
BO
SETA
B­
Tri
1112,
Tetra
0.0000
0.0000
.
17924366.0000
0.0000
0.0000
15575979.0000
0.0000
0.0000
0.0000
234207.0469
5202291.5000
0.0000
0.0000
­
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
Totals
Unknowns
127603
0.0000
Named
l
.
30240096
100.0000
,s­.

L
c
.
.

l
Intens
I
ty
(rnV1
.

,

k=­
.

.

B­
Tr
I
[T&
MINAI&
l91
BTR2531JLOllb19,1,1
*
Reported
on
25­
JUL­
2001
at
19:
41
,
Page
2
30367700
100.0000
ANALYSIS
SUMMARY
.
.

Method..........................
B­
TRI
Run
sequence....................
B­
TRI
Calibration.....................
B­
TRI
Normalised
%
calibration
using
area
Calibration
last
modified
on
25­
JUL­
2001
at
19:
07
Method
last
modified
on
11­
JAN­
2001.
at
15:
34
Uncalibrated
peaks
use
user
factor
(0.0000)
.

.

l
.
.

L
t
.

w
­

.