Document ID: EPA-HQ-OPPT-2002-0066-0023
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2002-12-05T05:00Z

United
States
Offtce
of
EPA­
560/
5­
86­
036
Environmental
Protection
Toxic
Substances
December.
1986
Agency
Washington
DC
2046G
Toxic
Substances
SEPA
BROAD
SCAN
ANAbYStS
OF
THE
FY82
NATIONAL
HUMAN
ADIPOSE
TISSUE
SURVE 
SPECIMENS
VOLUME
II
­
VOLATILE
ORGANIC
C
MPOUNI
0P?
7­
2wz­
QO
66­
002
3
REPROWCEOBY
US.
DEPARTMENTOFCOMMERCE
HAfloNplLrrcHMcAL
000001
INFFORMATIONSEWNICE
SPRINGFELD.
VA22161
PREFACE
This
report
is
the
second
of
a
five­
volume
series
that
details
the
broad
scan
chemical
analysis
of
composite
adipose
tissue
samples.
These
composite
samples
were
prepared
from
individual
specimens
obtained
from
the
Environmental
Protection
Agency's
(
EPA)
National
Human
Adipose
Tissue
Survey
(
NHATS)
fiscal
year
1982
(
FY82)
repository.
­.
....
.

This
volume
summarizes
data
generated
from
the
analysis
of
the
composited
samples
for
volatile
organic
compounds.
Volume
I,
the
executive
summary
presents
a
synopsis
of
a71
analysis
efforts
completed
under
the
broad
scan
program.
Volumes
I11
through
V
deal
specifically
with
the
chemical
analy
sis
of
the
NHATS
composites
for
general
semivolatile
organic
compounds,
polychlorinated
dibenzo­
e­
dioxins
(
PCDD),
and
dibenzofurans
(
PCDF),
and
trace
elements
The
statistical
analyses
of
the
data
reported
in
these
volumes
will
be
reported
separately
by
the
EPA's
Office
of
Toxic
Substances
(
OTS)
Design
and
Development
Branch
contractor,
Battelle
Columbus
Laboratories.

The
entire
series
of
reports
are
referenced
as
follows:
Stanley
JS.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
I:
Executive
summary.
 PA
560/
5­
86­
035.
Stanley
JS.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
11:
Volatile
organic
compounds.
EPA
560/
5­
86­
036.
Stanley
JS.
1986.
Broad
scan
analysis'of
human
adipose
tissue:
Volume
111:
Semivolatile
organic
compounds.
EPA
560/
5­
86­
037.
Stanley
35..
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
IV:
Polychlorinated
dibenzo­
p­
dioxins
(
PCDD)
and
polychlorinated
dibenzofurans
(
PCDF).
 PA
560/
5­
86­
038.

­
Stanley
JS,
Stockton
RA.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
V:
Trace
elements.
EPA­
560/
5­
86­
039.

These
method
development,
sample
analyses,
and
reporting
activities
were
completed
for
the
EPA/
OTS
Field
Studies
Branch
(
FSB)
broad
scan
analysis
of
human
adipose
tissue
program
(
EPA
Prime
Contract
Nos.
68­
02­
3938and
68­
024252
Work
Assignments
8
and
21,
respectively,
Ms.
Janet
Remmers,
Work
Assignment
Manager,
and
Dr.
Joseph
Breen,
Project
Officer).

The
samples
were
prepared
with
the
assistance
of
Ms.
Leslie
Moody
and
Mr.
Steven
Turner.
The
HRGC/
MS
methods
development
and
sample
analyses
were
conducted
by
Mr.
Steven
Turner,
Ms.
Margaret
Wickham,
and
Mr.
Gil
Radolovich.
The
cornpositing
scheme
used
to
prepare
the
samples
from
the
NHATS
repository
was
provided
by
Dr.
Gregory
Mack,
Battelle
Columbus
Laboratories,
under
contract
to
the
EPA/
OTS
Design
and
Development
Branch
(
Mr.
Philip
Robinson,
Task
Manager,
and
Ms.
Cindy
Stroup,
Program
Manager).

MIDWEST
RESEARCH
INSTITUTE
.
AhnE.
Going
Paul
C.
Constant
Director
Program
Manager
Chemical
Sciences
Department
iii
088002
DISCLAIMER
i
This
document
has
been
reviewed
and
approved
for
publication
by
the
Office
of
Toxic
Substances,
Office
of
Pesticides
and
Toxic
Substances,
U.
S. 
Environmental
Protection
Agency.
The
use
of
trade
names
or
commercial
products
does
not
constitute.
Agency
endorsement
or
recommendation
for
use.
i
...*

TABLE
OF
CONTENTS
Pagc!

Executive
Summary
..........................
xi
1.
I
ntroducti.
on
........................
1
A
.
Broad
Scan
Analysis
Strategy
...........
1
B.
Work
Assignment
Objectives
.............
1
C.
Background
Information
...............
2
I1.
Recommendations
.......................
3
111
Experimental........................
3
A
.
 3­
C
.

0.

E.

F.
G.

H
.
Collection
and
Storage
of
NHATS
Specimens.....
4
Sample
Compositing
Activity.............
4
Sources
and
Preparation
of
Analytical
Reagents
.
.
5
1.
Internal
Quantitation
Standards
.......
5
2
.
Reference
Compounds
.............
6
3
.
Spiking
Solutions
..............
7
Apparatus
....................
8
1.
Dynamic
Headspace
Purge
and
Trap
System
...
8
2
.
High
Resolution
Gas
Chromatography/
Mass
.
Spectrometry
................
8
Analysis
Procedures................
10
1.
Spiking
Procedure
..............
10
2.
Method
Blank
Analysis
............
10
3
.
Calibration
Curves
for
Reference
Standards.
.
10
4
.
Composited
Sample
Analysis..........
11
Quality
Control
Procedures
............
11
Data
Interpretation................
11
1..
Qualitative
Identification..........
11
2.
Quantitation.................
14
Method
Val
idation.................
14
IV
.
Resu1
ts
..........................
23
V
.
Quality
Assurance/
Quality
Control
.............
75
A
.
Instrument
Performance
Checks...........
75
1.
Internal
QC
.................
75
2.
External
QC
...........
....
75
8.
Spiked
Adipose
Tissue
Samples......
....
76
C.
Internal
Standards
..........
....
76
VI
.
References...................
.....
a5
Append
x
A
.
Analyticat
Method
for
the
Determination
of
Vo
ati
le
Organic
Compounds
in
Human
Adipose
Tissue.
.
.....
A­
1
Amendix
8
.
Volatile
Organic
Compound
Data
from
the
NHATS
FY82
..
Composite­
Human
Adipose
Tissue
Samples
........
 3­
3
Appendix
C
.
Cornpositing
Scheme
for
the
NHATS
FY82
Specimens.....
c­
1
V
00Q004
Preceding
page
blank
LIST
06
FIGURES
Figure
Page
1
Schematic
of
apparatus
for
volatile
organic
analysis
...
9
.2
Analytical
scheme
for
analysis
of
volatile
organic
compounds
from
human
adipose
tissue.
.........
12
.

3
Purging
efficiency
of
three
internal
standards
(
1
pg
each)
from
20
g
of
human
adipose
tissue,
over
four
sequential,
40­
min
heating
and
purging
cycles.
.....
19
4
Purging
efficiency
of
eight
stable
isotope
labeled
internal
standards
(
1pg
each)
from
20
g
of
human
adipose
tissue
over
four
sequential
40­
min
heating
and
purging
cycles
...................
20
­
5
Purging
efficiency
of
seven
target
analytes
(
0.20
pg
each)
spiked
into
20
g
of
human
adipose
tissue,
over
four
sequential
40­
min
heating
and
purging
cycles.
...
21
Purging
efficiency
of
six
target
analytes
(
0.20
pg
each)
spiked
into
20
g.
of
human
adipose
tissue,
over
four
sequential
40­
min
heating
and
purging
cycles
......
22
Comparison
of
purging
efficiencies
for
target
analyte/
deuterated
analog
pairs:
(
a)
benzene/
d,­
benzene
and
(
b)
toluene/
d,­
toluene
....................
24
Comparison
of
purging
efficiencies
for
target
ana?
yte/
deuterated
analog
pairs:
(
a)
chlorobenzene/
d5­
chlorobenzene
and
(
b)
ethylbenzene/
d,,­
ethylbenzene.
..
25
Comparison
of
purging
efficiencies
for
target
analyte/
deuterated
analog
pairs
for
(
a)
1,1,2,2­
tetra­
chloroethane/
d2­
l,
l,
2,
Z­
tetrachloroethane
and
(
b)
1,2­
dich10robenzene/
d4­
1,4­
dich10robenzene
.....
26
10
Purging
efficiency
of
seven
volatile
organic
analytes
.
endogenous
to
human
adipose
tissue
over
four
sequential
40­
min
heating
and
purging
cycies
......
27
11
HRGC/
MS
chromatogram
of
purge
tower
standard
analyzed
daily
to
document
instrument
performance
........
28
12
HRGC/
MS
chromatogram
for
the
volatile
organic
analysis
of
a
bulk
adipose
(
tissue
standard)
spiked
with
1.0
pg
of
each
internal
standard
and
0.20
pg
of
each
target
analyte.
........................
29
13
HRGC/
MS
chromatogram
of
volatile
compounds
from
the
NHATS
FY82
composite
of
the
0­
14yr
age
group
from
the
Middle
Atlantic
census
division.
............
30
vii
Precedingpage
blank
OQIQOBS
LIST
OF
FIGURES
(
concluded)

Figure
Page
14
Comparison
of
the
HRGC/
MS
chromatograms
for
the
volatile
organic
analytes
for
three
composite
age
groups
from
the
Middle
Atlantic
census
division.
..........
31
15
Comparison
of
the
HRGC/
MS
chromatograms
for
the
volatile
organic
a.
nalytes'for
three
composite
age
groups
from
the
East
North
Central
census
division
...........
32
16
Comparison
of
the
HRGC/
MS
chromatograms
of
the
volatile
organic
analysis
of
three
composite
specimens
repre­
senting
the
15­
44
age
group
from
three
census
divisions.
33
17
Comparison
of
the
HRGC/
MS
chromatograms
of
the
vol
atile
organic
analysis
of
three
composite
specimens
repre­
senting
the
0­
14
age
group
from
three
census
divisions
.
34
18
Incidence
of
detection
of
volatile
organic
compounds
in
cornposited
human
adipose
tissues
from
the
Northeast
census
region.
.....................
36
19
Incidence
of
detection
of
volatile
organic
compounds
in
cornposited
human
adipose
tissues
from
the
South
census
region.
.....................
37
20
Incidence
of
detection
of
volatile
organic
compounds
in
cornposited
human
adipose
tissues
from
the
North
Central
census
region.
.....................
38
21
Incidence
of
detection
of
volatile
organic
compounds
in
composited
human
adipose
tissues
from
the
West
census
region.
.....................
39
2.2
Observed
HRGC/
MS
responses
for
the
internal
standards
d­
chloroform
and
d6­
benzene,
from
method
blanks,
spiked
tissue
samples
and
the
NHATS
composite
samples.
.
81
23
Observed
HRGC/
MS
responses
for
the
internal'
standards
d8­
toluene
and
d,­
chlorobenzene,
from
method
blanks,
spiked
tissue
samples
and
the
NHATS
composite
samples.
..
82
24
Observed
HRGC/
MS
responses
for
the
internal
standards
dIo­
p­
xylene
and
d,
o­
ethylbenzene,
from
method
blanks,
spiked
tissue
samples
and
the
NHATS
composite
samples.
.
a3
25
Observed
HRGC/
MS
responses
for
the
internal
standards
d2­
1,
l,
2,2­
tetrachloroethane
and
d4­
dichlorobenzene,
from
method
blanks,
spiked
tissue
samples
and
the
NHATS
composite
samples.
................
84
viii
.
LIST
OF
TABLES
Table
Page
­
1
Characteristic
Ions,
Internal
Standards,
and
Relative
Retention
Times
Used
to
Identify
and
Quantitate
Target
Analytes.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
13
2
Summary
of
Spiked
Recovery
(
X)
Experiments
for
Volatile
Analytes
from
20
g
of
Human
Adipose
Tissue
.
.
.
.
.
.
.
16
3
Summary
of
Spiked
Recovery
(%)
Experiments
Based
on
a
Single
Internal
Standard
Bromoch?
oropropaneversus
Multiple
Deuterated
Standards
(
Isotope
Dilution)
­.
.
.
17
4
Data
Report
­
Chloroform
(
CAS
No.
67­
66­
3)
­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
.
.
.
.
.
.
40
5
Data
Report
­
l,
l,
l­
Trichloroethane
(
CAS
No.
67­
66­
3)­
FY82
Composite
Adipose
Tissue
Samp les.
.
.
.
.
.
.
.
.
.
42
6
Data
Report
­
Bromodichloromethane
(
CAS
No.
75­
27­
4)
­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
.
.
.
­.
.
44
7
Data
Report
­
Benzene
(
CAS
No.
71­
43­
2)­
FY82
Composite
Adipose
Tissue
Samples.
.
­.
.
.
.
.
.
.
.
46
8
Data
Report
­
Tetrachloroethene
(
CAS
No.
127­
18­
4)
­
FY82
Compbsite
Adipose
Tissue
Samples.
­.
.
.
.
.
.
.
.
48
3
Data
Report
­
Dibromochloromethane
­
FY82
Composite
Adipose
Tissue
Samples.
. .
.
.
.
.
.
.
.
50
10
Data
Report
­
l,
I,
Z­
Trichloroethane
(
CAS
No.
79­
00­
5)
­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
.
.
.
.
.
.
52
11
Data
Report
­
Toluene
(
CAS
No.
188­
88­
3).­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
.
.
­.
.
.
54
12
Data
Report
­
Chlorobenzene
(
CAS
No.
108­
90­
7)
­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
.
­.
.
.
.
56
13
Data
Report
­
Ethylbenzene
(
CAS
No.
100­
41­
4)
­
FY82
Composite
Adipose
Tissue
Samples.
­.
.
.
.
.
.
.
58
14
Data
Report
­
Bromoform
(
CAS
No.
75­
25­
2)
­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
.
,
.
.
.
.
60
15
Data
Report
­
Styrene
(
CAS
No.
100­
42­
5)
­
FY82
Composite
Adipose
Tissue
Samples.
_..
­.
.
.
.
.
.
62
16
Data
Report
­
1,1,2,2­
Tetrachl.
oroethane
(
CAS
No.
79­
34­
5)
­
FY82
Composite
Adipose
Tissue
Samples.
.
.
.
­.
.
.
­
64
ix
LIST
OF
TABLES
(
concluded)

Table
Page
­
17
Data
Report
­
1,2­
Dichlorobenzene
(
CAS
No.
95­
50­
1)
­
FY82
Composite
Adipose
Tissue
Samples.
..........
66
18
Data
Report
­
1,4­
Dichlorobenzene
(
CAS
No.
106­
46­
7)
­
FY82
Composite
Adipose
Tissue
Samples.
.........
68
19
Data
Report
­
Ethyl
Phenol
(
CAS
No.
25429­
37­
2)
­
FY82
Composite
Adipose
Tissue,
Samples.
.........
70
20
Data
Report
­
Xylene
(
CAS
No.
1330­
20­
7)
­
FY82
Composite
Adipose
Tissue
Samples.
.........
72
21
Incidence
of
Detection
of
Selected
Volatile
Organic
Compounds
in
the
NHATS
FY82
Composite
Samples.
.....
74
22
Summary
of
the
Internal
QC
Instrument
Performance
Checks
for
Selected
Volatile
Organic
Analytes
.........
77
23
Average
Recovery
for
InternaJ
QC
Instrument
Performance
Checks
.........................
78
24
Summary
of
Results
­
QC
Performance
Audit
Samples.
....
79
.25
Summary
of
Method
Recovery
(%)
of
Selected
Volatile
Organic
Analytes
Spiked
into
20­
9
Aliquots
of
Human
Adipose
Tissue
­
Internal
QC
...........
80
X
000008
EXECUTIVE
SUMMARY
The
U.
S.
Environmental
Protection
Agency's
Office
of
Toxic
Substances
(
EPA/
OTS)
maintains
a
unique
program
for
monitoring
human
exposure
to
potentially
toxic
substances.
The
National
Human
Adipose
Tissue
Survey
(
NHATS)
is
a
statistically
designed
annual
program
to
collect
and
analyze
a
nationwide
sample
of
adipose
tissue
specimens
for
toxic
compounds.
The
primary
focus
for
NHATS
has
been
to
document
trends
in
human
exposure
to
environmentally
persistent
contaminants,
specifically
organochlorine
pesticides
and
polychlorinated
biphenyls
(
PCBs).

EPA/
OTS
has
recognized
the
need
to
provide
a
more
comprehensive
assessment
of
the
toxic
substances
that
accumulate
in
adipose
tissue.
Thus,
the
NHATS
specimens
collected
during
fiscal
year
1982
(
FY82)
were
designated
for
"
broad
scan
analysis''
to
determine
volatile
and
semivolatile
organic
compounds
and
trace
elements.

This
volume
of
the
final
report
deals
specifically
with
the
measurement
of
volatile
organic
chemicals
in
composited
adipose
tissue
specimens
from
the
FY82
NHATS
repository.
The
objectives
of
this
part
of
the
study
were
(
1)
to
develop
an
analytical
method
based
on
high
resolution
gas
chromatography/
mass
spectrometry
(
HRGC/
MS)
for
determination
of
volatile
organic
chemicals
in
human
adipose
tissue
and
(
2)
to
complete
the
analysis
of
the
FY82
NHATS
specimens
as
composited
for
volatile
organic
compounds.

The
analytical
method
developed
to
sample
volatile
organic
compounds
from
human
adipose
tissue
is
based
on
a
heated
dynamic
headspace
purge
and
trap
technique.
The
volatile
organic
compounds
were
separated
and
detected
using
HRGC/
MS.
HRGC
was
selected
to
achieve
the
best
possible
separation
of
volatile
components,
and
MS
was
selected
to
provide
the
necessary
specificity
to
identify
positively
the
volatile
compounds
present
in
the
tissue.
Target
analytes
were
quantitated
based
on
a
multiple
internal
standard
technique.
The
method
evaluation
studies
and
daily
quality
control
checks
demonstrated
'
that
method
accuracy
was
improved
for
analytes
which
had
a
corresponding
deuterated
analog
as
an
internal
quantitation
standard.

Forty­
six
composite
samples
were
prepared
from
the
FY82
NHATS
repository
according
to
a
study
design
prepared
by
the
EPA/
OTS
Design
and
Development
Branch
contractor,
Battelle
Columbus
Laboratories.
The
composite
samples
represent
the
nine
U.
S.
cen~
usdivisions,
stratified
by
three
age
groups
(
0­
14,15­
44,
and
45
plus).

The
HRGC/
MS
analysis
of
the
volatile
compounds
purged
from
the
human
adipose
demonstrated
a
complex
mixture
of
compounds
consisting
primarily
of
a?
dehydes,
ketones,
hydrocarbons,
and
carboxylic
acid
esters.
Additional
corn­
pounds
classified
as
aromatic,
halogenated
aliphatic,
and
halogenated
aromatic
.
compounds
were
detected
as
minor
constituents.

Quantitative
efforts
focused
on
target
analytes
classified
as
priority
pollutants.
Quantitative
data
are
reported
for
17
specific
compounds.
The
predominant
target
analytes
noted
included
chloroform,
l,
l,
l­
trichloroethane
benzene,
tetrachloroethene,
toluene,
chlorobenzene,
ethylbenzene,

xi
080089
styrene,
1,1,2,2!­
tetrachloroethane,
1,4­
dichlorobenzene,
1,2­
dichlorobenzene,
xylenes,
and
ethyl
phenol.
In
all
composite
samples
several
compounds
were
detected
including
styrene,
the
xylene
isomers,
1,4­
dichlorobenzene,
and
ethyl
phenol.
The
frequencies
of
detection
for
each
of
the
compounds
by
age
groups
and
census
divisions
are
detailed
in
the
report.
The
volatile
organic
compounds
were
detected
in
the
composites
from
all
census
divisions
and
age
group.

The
quantitative
data
for
the
17
specific
compounds
have
been
submitted
along
with
all
supporting
quality
control
data
to
the
OTS
design
and
development
contractor,
Battelle
Columbus
Laboratories,
for
statistical
analysi
s.

Characterization
of
additional
chromatographic
peaks
in
the
HRGC/
MS
data
to
identify
other
compounds
of
interest
to
the
Agency
has
been
initiated
under
a
separate
work
assignment
(
Contract
No.
68­
02­
4252,
Work
Assignment
No.
23).

xi
i
I.
INTRODUCTION
The
National
Human
Adipose
Tissue
Survey
(
NHATS)
is
the
main
operative
program
of
the
National
Human
Monitoring
Program.
The
National
Human
Monitoring
Program
was
first
established
by
the
U.
S.
Public
Health
Service
in
1967
and
was
subsequently
transferred
to
the
U.
S.
Environmental
Protection
Agency
(
EPA)
in
1970.
During
1979
the
program
was
transferred
within
EPA
to
the
Exposure
Evaluation
Division
(
EED)
of
the
Office
of
Toxic
Substances
(
OTS).

NHATS
is
an
annual
program
to
collect
a
nationwide
sample
of
adipose
tissue
specimens
and
to
chemically
analyze
them
for
the
presence
of
toxic
compounds.
The
objective
of
the
NHATS
program
is
to
detect
and
quantify
the
prevalences
of
the
compounds
in
the
general
population.
The
NHATS
data
are
used
to
address
part
of
OTS's
mandate
under
the
Toxic
Substances
Control
Act
(
TSCA)
to
assess
chemical
risk
to
the
U.
S.
population.
The
specimens
are
collected
from
autopsied
cadavers
and
surgical
patients
according
to
a
statistical
survey
design
(
Lucas,
Pierson,
Meyers,
Handy
1981).
The
survey
design
ensures
that
specified
geographical
regions
and
demographic
categories
are
appropriately
represented
to
permit
valid
and
precise
estimates
of
baseline
'
levels,
time
trends,
and
comparisons
across
subpopulations.

The
data
for
the
NHATS
are
generated
by
collecting
and
chemically
anafyzing
adipose
tissue
specimens
for
selected
toxic
substances.
Historically
organochlorines
and
polychlorinated
biphenyls
(
PCBs)
have
been
selected
for
evaluation.

A.
Broad
Scan
Analysis
Strategy
*

EPA/
OTS
has
recognized
the
need
to­
provide
a
more
comprehensive
assessment
of
the
toxic
substances
that
accumulate
in
adipose
tissue.
An
aggressive
strategy
to
assess
TSCA­
related
substances
that
persist
in
the
adipose
tissue
of
the
general
U.
S.
population
has
been
developed
by
 ED.
The
NHATS
specimens
col7ected
during
fiscal
year
1982
(
FY82)
were
selected
for
a
broad
scan
analysis
of
volatile
and
semivolatile
organic
TSCA­
related
chemicals
and
trace
'
elements
(
Mack,
Stanley
1984).

The
initiative
to
achieve
a
more
comprehensive
assessment
necessitated
either
the
development
of
new
methods
or
the
modification
of
the
existing
analytical
procedures,
specifically
high
resolution
gas
chromatography/
mass
spectrometry
(
HRGUMS).
Data
on
organochlorine
pesticides
and
PCBs
reported
for
the
NHATS
specimens.
up
to
the
FY82
collection
are
based
on
packed
column
gas
chromatography/
electron
capture
detector
(
PGC/
ECD)
analysis.

8.
Work
Assignment
Objectives
The
objectives
of
this
phase
of
the
work
assignment
were
(
1)
to
identify
appropriate
analytical
methods
for
a
broad
scan
analysis
of
volatile
organic
compounds
in
human
adipose
tissue
based
on
HRGC/
MS
detection;
(
2)
to
conduct
preliminary
evaluation
of
the
analytical
procedures,
and
(
3)
to
complete
the
sample
workup
and
HRGC/
MS
analysis
of
46
composite
samples
prepared
from
the
NHATS
specimens
collected
during
FY82.
The
target
detection
range
far
analytes
by
the
HRGC/
MS
as
specified
in
the
current
NHATS
strategy
(
Mack,
Stanley
1984)
was
0.05
to
0.10pg/
g­
C.
Background
Information
The
exposure
of
the
general
U.
S.
population
to
volatile
organic
compounds
has
not
previously
been
addressed
through
a
national
sampling
of
b.
iologica1
matrices
(
breath,
blood
or
tissue).
Specific
studies
have
been
conducted,
however,
to
determine
the
effects
of
exposure
to
chemical
solvents,
monomers
such
as
vinyl
chloride
and
styrene
in
the
plastics
industry,
and
anesthetics
(
Wolff
1976;
Wolff,.
Loumer,
Selikoff,
Aubrey
1977;
Engstrom,
Riihimaki
1979;
Engstrom
1984).

The
fact
that
blood
and
breath
levels
of
volatile
organics
can
be
detected
at
declining
levels
from
several
hours
to
several
days
after
a
specific
exposure
incident
indicate
tissue
retention
(
Whitcher,
Cohen,
Trudell
1971;
Corbett
1973;
Wolff
1976).
Human
adipose
tissue
has
been
evaluated
as
a
depot
for
storage
and
release
of
volatiles
in
specific
exposure
studies
of
workers
to
styrene
and
ethylbenzene
in
the
polymerization
industry
(
Wolff
1976;
Wolff,
Daum,
loumer,
Selikoff,
Aubrey
1977;
Engstrom
1984).

Several
analytical
procedures
have
been
developed
for
the
measurement
of
specifjc
compounds
from
these
exposure
scenarios,
Analytical
techniques
have
required
dissolution
of
milligram
quantities
of
adipose
into
carbon
disulfide,
or
other
suitable
solvent,
followed
by
direct
injection
onto
gas
chromatographic
(
GC)~
columnswith
flame
ionization/
electron
capture,
microcoul
ometri
c
or
mass
spectrometer
(
MS)
detectors.
Other
analytical
procedures
combined
with
these
detection
systems
have
included:
(
a)
static
head­
space
analysis
of
heated
tissue,
(
b)
stripping
volatiles
from
heated
tissue
by
flowing
an
inert
gas
directly
through
the
rendered
sample,
(
c)
vacuum
distillation
and
cryogenic
focusing
of
the
analytes
on
a
high
resolution
gas
chromatography
(
HRGC)
column,
and
(
d)
dynamic
solution
purge
and
trap
and
headspace
analysis
of
heated
tissue
water
mixtures
combined
with
cryogenic
focusing
and
HRGC
analysis.
Each
of
these
techniques
has
certain
advantages
and
disadvantages
in
terms
of
complexity
of
the
actual
sampling
procedure
and
sensitivity
and
selectivity
of
the
detector
(
Novotny,
McConnell,
Lee,
Farlow
1974;
Politzer,
Githens,
Dowty,
Laseter
1975;
Luskus,
Kilian,
Lackey,
Biggs
1977;
Snyder,
Erlichman,
Goldstein,
Laskin
1977;
Karbowski,
Braun
1978;
Peoples,
Pfaffenberger,
Enos,
Shafik
1978;
Balkon,
Leary
19a;
Peoples,
Pfaffenberger, 
Shafik,
Enos
1979;
Pfaffenberger,
Freal
1979;
Michael,
Erickson,
Parks,
Pellizzari
1980;
Pantarotto,
Fanelli,
Belletti,
Bidoli
1980;
Reddrop,
Riess,
Slater
1980;
Vogt,
Liao,
Sun
1980;
Zuccato,
Marcucci,
Mussini
1980;
Lin,
Fu,
Bruckner,
Feldman
1982;
Hiatt
1981;
Reinert,
Hunter,
Sabatino
1983).

An
analytical
method
for
the
measurement
of
volatile
organic
chemicals
in
human
adipose
tissue
has
been
developed
as
a
result
of
this
work
assignment.
This
analytical
method
is
a
modification
of
a
dynamic
headspace
purge
and
trap
procedure
(
Michael,
Erickson,
Parks,
Pellizzari
1980)
combined
with
high
resolution
gas
chromatography
and
mass
spectrometry.
This
report
describes
the
method
and
summarizes
the
volatile
organic
data
for
46
composite
specimens
from
the
FY82
NHATS
repository
determined
with
the
method.

Following
this
introductory
section,
Section
I1
presents
recommendations
for
further
activities
for
volatile
organics.
Section
III
is
the
2
QQ(
BO3.2
experimental
section
and
describes
the
coliection
and
storage
of
the
NHaTS
specimens,
the
adipose
tissue
cornpositing
procedures,
the
development
of
the
analytical
method,
and
the
routine
analytical
procedures.
Section
IV
presents
the
results
of
the
composite
tissue
analyses.
Section
V
summarizes
the
quality
control
(
QC)
procedures
and
results.
Section
VI
contains
references.
Appendices
A,
E,
and
C
provide,
respectively,
the
volatile
organic
analysis
method
in
detail,
additional
data
tables
on
the
results
of
the
analyses,
and
the
exact
compositing
scheme
used
for
the
FY82
NHATS
specimens.

Ir
­
RECOMMENDATIONS
Further
analytical
development
should
be
pursued
to
improve
the
determination
of
volatile
organic
compounds
in
human
adipose
tissue
samples.
These
improvements
should
specifically
include
smaller
sample
sizes
(
1.0
to
5.0g),
more
efficient
transfer
of
volatile
organics
onto
the
HRGC*
column,
and
further
development
of
the
isotope
dilution
quantitation
technique.
These
modifications
can
possible
be
achieved
by
using
widebore
HRGC
column's
and/
or
cryofocusing
techniques.

The
analytical
method
should
be
modified
to
provide
quantitative
information
on
compounds
of
greater
volatijity
than
chloroform
(
such
as
methylene
chloride,
vinyl
chloride,
etc.).
This
possibly
could
be
accomplished
by
conducting
two
analyses
on
each
tissue
sample.
The
first
analysis
should
be
conducted
for
the
more
volatile
compounds
with
the
sample
heated
in
the
range
of
50­
8OoC
and
the
headspace
sampled
for
15
min
or
less.
The
second
sample
analysis
should
be
conducted
with
the
procedures
specified
in
this
report
to
provide
quantitative
data
for
compounds
ranging
in
volatility
from
­
chloroform
through
the
dichlorobenzene
isomers.

Stability
studies
should
be
conducted
to
determine
the
effects
of
long­
term
storage
at
subzero
temperature,
and
repeated
thawing
and
freezing
on
the
integrity
of
the
volatile
organic
content
in
the
sample.
The
results
of
the
sample
analysis
conducted
for
the
FY82
composites
indicate
considerable
differences
in
the
absolute
quantities
of
the
major
volatile
constituents
(
hydrocarbons,
aldehydes,
ketones,
etc.)
for
samples
analyzed
within
6
mo
of
collection
and
the
NHATS
specimens
that
have
been
archived
prior
to
analysis
for
up
to
2
yr.

I1I.
EXPERIMENTAL
This
section
of
the
report
describes:

A.
collection
and
storage
of
NHATS
specimens;
8.
sample
compositing
activity;
c.
sources
and
preparation.
of
analytical
standards;
­
D.
apparatus;
E.
analysis
procedures;
.
F.
quality
control
procedures;
G.
data
interpretation;
and
H.
method
validation.

3
.

A.
Collection
and
Storage
of
NHATS
Specimens
The
adipose
specimens
were
.
originally
collected
during
FY82
(
October
1,
1981,
through
September
30,
1982)
for
determination
of
organic
chlorine
pesticide
and
PCB
residues.
The
specimens
were
col?
ected
during
surgical
procedures
or
as
part
of
postmortem
examinations.
The
cooperating
physicians
and
pathologists
were
requested
to
acquire
at
least
5
g
of
high
lipid
adipose
(
subcutaneous,
perirenal,
or
mesenteric),
taking
precautions
to
avoid
Contamination
that
might
result
in
direct
contamination
from
chemicals
such
as
solvents,
paraffin,
disinfectants,
preservatives,
or
plastics.
The
cooperators
were
given
no
specific
instructions
to
avoid
potential
contamination
that
might
arise
from
background
contribution
of
solvents
or
metals.

The
adipose
tissue
specimens
were
sealed
in
glass
jars
and
frozen
'

(­
20OC)
following
collection.
The
specimens
were
shipped
in
insulated
coolers
packed
on
dry
ice.
The
FY82
specimens
were
originally
received
and
stored
at
EPA's
Toxicant
Analysis
Center
(
TAC)
at
Bay
St.
louis,
MS.
The
NHATS
repository
was
transferred
to
Midwest
Research
Institute
(
MRI)
during
September
1982.
The
specimens
were
shipped
in
insulated
coolers
and
packed
on
dry
ice.
The
specimens
were
inventoried
at
MRI
upon
receipt
and
were
then
stored
in
freezers
(­
20OC).
Precautions
were
taken
to
ensure
that
the
specimens
remained
frozen
during
all
inventory
and
sample
handling
procedures.

8.
Sample
Compositing
Activity
The
NHATS
FY82
adipose
tissue
specimens
were
subsampled
and
composited
as
specified
by
EPA's
Design
and
Development
Branch
contractor,
Battelle
Columbus
Laboratories
(
BCL).
Prior
to
preparation
of
the
composites,
all
of
the
FY82
specimens
were
retrieved
from
the
NHATS
repository
and
the
individual
specimens
bott?
es
were
grouped
according
to
the
designated
cornpositing
scheme
provided
by
BCL.
Care
was
taken
to
ensure
that
the
specimens
were
not
allowed
to
reach
room
temperature.
The
specimen
were
stored
on
dry
ice
during
this
process
and
were
returned
to
a
freezer
(­
20
°
)
once
all
individual
specimen
for
a
specific
composite
had
been
located.

All
specimens
for
a
specific
composite
were
removed
from
the
freezer
at
the
same
time
for
the
cornpositing
effort.
The
specimens
were
placed
on
dry
ice
so
they
would
remain
frozen
during
the
cornpositing
effort.
Each
specimen
was
handled
separately
and
each
was
subsampled
for
the
composites
for
both
volatile
and
semivolatile
organic
anlaysis.
This
resulted
in
minimum
handling
of
each
specimen.
Once
the
speciment
had
been
subsampled
for
each
composite
it
was
placed
on
dry
ice.
After
all
specimen
had
been
added
to
the
composites,
the
batch
was
returned
to
the
freezer.

All
samples
were
handled
in
a
positive
pressure
Plexiglas
hood
of
approximately
94.5
L
volume
to
prevent
contamination
from
laboratory
air.
Compressed
air
was
filtered
through
a
charcoal
trap
to
remove
potential
volatile
contaminants
from
air
supply
before
it
entered
the
hood.
The
subsamples
were
manipulated
with
the
rounded
end
of
a
lab
spoon­
type
stainless
steel
spatulas
and
placed
in
40­
mL
vials
with
TFE
septa
caps.
Each
specimen
was
manipulated
with
a
separate
clean
spatula.
All
weighings
were
performed
to
k
0.1
g
on
a
Mettler
open
pan
balance
placed
in
the
hood.

4
.~
.
..
..
'
3
3'.

The
nominal
mass
of
each
individual
specimen
necessary
to
achieve
a
final
composite
mass
of
20
g
was
determined
before
proceeding
with
the
physical
compositing.
For
example,
if
a
composite
consisted
of
20
specimens,
1.0g
of
each
specimen
was
necessary
to
achieve
a
final
composite
mass
of
20
g­
Separate
composite
samples
were
prepared
for
both
semivolatile
(
Stanley
1986c)
and
volatile
organic
analysis.
The
individual
specimens
were
added
first
to
the
composites
for
the
semivolatile
organic
analysis.
This
resulted
in
the
addition
of
a
total
available
specimen,
in
some
cases,
to
the
semivolatile
organic
composite
only.
As
a
result,
several
of
the
volatile
organic
composites
contain
somewhat
less
than
the
target
20
g
of
tissue
mass.
The
samples
resulting
from
the
46
volatile
organic
composites
ranged
from
5.1
to
25.6
g
total
mass
with
an
average
mass
of
19
g.
Appendix
C
provides
a
summary
of
the
exact
compositing
scheme
for
both
the
volatile
and
semivolatile
organic
analyses.

Prior
to
the
compositing
effort,
the
vials
were
washed
in
soap
and
water,
rinsed
thoroughly
with
tap
water,
deionized
water,
bulk
acetone,
Burdick
and
Jackson
(%&
J)
acetone,
and
B&
J
hexane,
and
then
placed
in
an
oven
at
200OC
for
48
h
before
use.
The
spatulas
were
washed
and
rinsed
as
above
and
were
dried
for
at
least
5
min
in
the
oven.

All
composites
were
stored
on
dry
ice
until
transfered
to
a
freezer
(­
20OC).
Before
being
placed
in
the
freezer
in
the
40­
ml
vials,
the
composited
samples
were
grouped
by
census
division
and
placed
in
1.0­
qt
jars
(
cleaned
as
above)
containing
a
layer
of
activated
charcoal
and
closed
with
a
TFE­
lined
cap.
The
samples
were
stored
in
the
freezer
until
analysis.

As
a
QA/
QC
check,
six
of
the
empty
vials
used
for
compositing
were
placed
in
the
hood
on
the
weighing
balance
for
approximately
15
min
(
approximating
the
time
needed
for
compositing),
and
then
were
capped,
sealed,
and
stored
with
the
samples.
These
blank
vials
were
included
with
the
analysis
of
the
composited
specimen
as
method
blanks.

The
samples
resulting
for
the
46
composites
ranged
from
5.1
to
25.6
g
total
mass
with
an
average
mass
of
19
g.
Appendix
C
provides
a
summary
of
the
exact
compositing
scheme.

C.
Sources
and
Preparation
of
Analytical
Reagents
The
sources
of
the
internal
standards
and
reference
compounds
and
the
procedures
for
preparing
spiking
and
calibration
standards
are
described
below.

1.
Internal
Quantitation
Standards
A
three­.
component
internal
quantitation
standard
mixture
was
obtained
from
Supelco,
lnc.
(
Catalog
No.
4­
8823,
Lot
No.
LA
11802).
This
mixture
contained
bromochloromethane,
1,4­
dichlorobutane,
and
1­
chloro­
Z­
bromopropane
at
20
mg/
mL
each
in
1.0mL
of
methanol.
This
mixture
was
used
as
received
and
was
stored
in
the
freezer
in
its
original
resealable
ampule.

5
080015
A
second
stock
solution
of
deuterated
internal
quantitation
standards
was
prepared
from
the
compounds
listed
below
by
aliquoting
each
with
a
100­
pL
syringe
into
a
IO­
mL
volumetric
flask
and
diluting
to
the
mark
with
methanol
(
B&
J
high
purity,
Lot
No.
43029).
The
volume
of
each
compound
necessary
to
achieve
the
desired
concentration
was
determined
by
the
density
of
the
specific
compound.
The
final
concentration
was
approximately
10
mg/
mL
for
each
deuterated
internal
standard.
Because
the
1,4­
d4­
dich1orobenzene
is
a
solid,
a
separate
stock
was
prepared
in
methanol
before
addition
to
the
solution
containing
the
other
deuterated
analogs.
The
final
mixture
was
sealed
in
two
5­
mL
vials
and
stored
in
the
freezer
until
just
prior
to
use.

Compound
d6­
benzene
d­
chloroform
l,
l,
Z,
Z­
d,­
tetrachloroethane
d,­
methylene
chloride
d5­
chlorobenzene
1,4­
d4­
dichlorobenzene
dIo­
ethylbenzene
de­
to1uene
d,,­
e­
xylene
2.
Reference
Compounds
Suppl
ier
Aldrich
Gold
Label
(
99.5%
0)
No.
15,
181­
5
Aldrich
Gold
Label
(
99.8%
D)
No.
15,
182­
3
M
and
D
Isotopes
No.
MD­
1416
M
and
D
Isotopes
No.
MD­
53
KOR
Isotopes
(
99%
DS)
NO.
521510
KOR
Isotopes
(
98%
D4)
No.
521530
KOR
Isotopes
(
98%
Dlo)
No.
521443
KOR
Isotopes
(
99.9%
D8)
No.
510041
KOR
Isotopes
(
98%
DIo)
No.
521133
Several
compounds
characteristic
of
aromatic
compounds,
chlorinated
and
brominated
a1
iphatic
compounds,
and
chlorinated
aromatic
compounds
were
selected
for
preparation
of
analytical
standards.
These
reference
compounds
were
also
selected
as
a
preliminary
list
of
target
analytes
as
a
result
of
their
presence
in
tissue
from
the
preliminary
method
development
and
their
classification
as
priority
pollutants.

The
compounds
listed
below
were
aliquotted
with
a
100­
pL
syringe
into
a
10­
mL
volumetric
flask
that
was
partially
filled
(
approximately
5
mL)
with
methanol.
The
volume
of
each
compound
necessary
to
achieve
the
desired
concentration
was
determined
from
the
density
of
each
specific
compound.
The
solution
was
diluted
to
the
mark
and
stored
in
the
same
manner
as
the
internal
quantitation
standard
solutions.
The
compounds
were
a1
iquotted
to
obtain
a
final
stock
concentration
of
approximately
IO
mg/
mL
for
each
compound.

Compound
bromoform
dibromochloromethane
to1uene
1,1,2­
trichloroethane
styrene
tetrachloroethylene
bromod
i
chl
oromethane
chlorobenzene
1,2­
dichlorobenzene
ethylbenzene
Supplier
Aldrich
Gold
Label
(
99%/
B
EtOH)
Columbia
No.
01843
B&
J
H.
P.
No.
A1­
857
Aldrich
No.
JB­
070177
(
95%)
Eastman
No.
1465
Aldrich
Gold
Label
No.
120457
Aldrich
No.
7628AH
(
98%)
Aldrich
No.
120277
(
99%)
Aldrich
No.
05­
680­
2
(
98%)
Aldrich
No.
E1­
250­
8
(
99%)

6
I
I
_,.
.­.
..
I.,,,
i .
c
...­,..
::,..
­,
,
.
i
,.
.
i.!
.
,

Compound
Supplier
1,1,2,2­
tetrachloroethane
 
Baker
No.
017386
l,
l,
l­
trichloroethane
Fisher
No.
775974
ch
1or0form
B&
J
H.
P.
(
XEtOH
preservative)
No,
AG594
benzene
MCB
Pest.
Grade
No.
U2738
carbon
disulfide
Mal
1i
nckrodt
No.
KMEE
3.
Spiking
Solutions
The
reference
stock
solution
and
the
two
internal
quantitation
standard
stock
solutions
(
Supelco
mixture
and
the
deuterated
analog
mixture)
were
.
used
to
make
up
the
spiking
solutions
necessary,
for
HRGC/
MS
analysis.
The
three
separate
stock
solutPons
allowed
manipulation
of
the
concentrations
of
the
spiking
levels
to
verify
method
calibration
and
accuracy
of
the
analyses
from
spiked
tissue
and
blank
samples.
,

­
Spiking
solutions
were
prepared
fresh
weekly
from
the
three
stock
solutions.
The
spiking
solutions
were
prepared.
in
1.0­
mL
microreaction
vials
(
Supelco
No.
3­
3292)
with
Mininert
Valves
(
Supelco
No.
3­
301).
Tetraglyme
was
used
as
the
solvent
for
the
spiking
solutions
to
enhance
their
stability.
All
spiking
solutions
were
stored
in
the
refrigerator
and
transported
between
the
GC/
MS
facility
and
the
laboratory
on
ice
in
a
cooler.
Following
sample
spiking,
the.
solutions
were
immediately
returned
to
the
cooler.

The
spiking
solutions
were
prepared
by
aliquoting
tetraglyme
into
the
1.0­
mt
reaction
vials
and
then
spiking
the
tetraglyme
with
the
stock
solutions
For
examp le,
a
500­
ng/
pL
internal
standard
spiking
solution
was
made
/
­
by
injecting
975
pL
of
tetraglyme
with
a
1.0­
mL
syringe
(
availab ie
from
Supelco,
Inc.)
into
the
reaction
vial
and
then
injecting
25.0
pL
of
the
three­
component
(
20
mg/
mL)
Supelco
internal
quantitation
standard
stock
solution
into
the
tetraglyme,
A
500­
ng/
vL
spiking
solution
of
the
deuterated
internal
­
standards
was
similarly
prepared
by
spiking
950
pL
of
tetraglyme
with
50.0
pL
of
the
10­
mg/
mL
deuterated
internal
standard
stock
solution.

The
target
analyte
spiking
solution
was
prepared
in
the
same
manner
but
at
100
ng/
pL.
This
was
accomplished
by
spiking
990
pL
of
tetraglyme
with
10.0
pL
of
the
target
analyte
stock
solution.

When
the
actual
sample
analyses­
were
initiated,
only
two
spiking
solutions
were
necessary.
A
500­
ng/
pL
solution
of
the
three
internal
standards
from
the
Supelco
mixture
and
the
nine
deuterated
internal
standards
were
combined.
This
mixed
internal
quantitation
standard
solution
was
prepared
with
925
pt
of
tetraglyme,
25.0
pt
of
the
three­
component
Supelco
standard,
and
50.0
pL
of
the
deuterated
internal
standard
stock
solution.
The
target
analyte
spiking
solution
was
prepared
at
the
100­
ng/
vL
level
as
described
above.

7
D.
Apparatus
.
The
design
of
the
dynamic
headspace
purge.
and
trap
system
used
to
collect
the
volatile
organics
and
the
HRGC/
MS
system
used
for
separating
and
identifying
these
compounds
are
described
below.

1.
Dynamic
Headspace
Purge
and
Trap
System
Method
development
for
volatile
organic
analytes
in
human
adipose
tiss
ue
led
to
the
system
shown
in
Figure
1.
Several
Wheaton
purge
and
trap
vessels
(
No.
991765)
were
modified
for
the
analyses.
The
thermometer
and
funnel
arms
were
cut
near
the
vessel
and
replaced
by
1/
4­
in.
Kovam
to
PX
seal
tubes.
(
Ace
Glass,
Inc.,
No.
PT.
976).
This
allowed
the
inlet
and
outlet
lines
to
be
connected
with
standard
1/
4­
in.
Swagelock@
fittings
and
provided
leak­
tight
connections.

The
Wheaton
vessel
was
connected
to
a
hot
water
circulating
bath
(
Haake,
No.
F4391)
maintained
at
95OC.
Approximately
5
min
was
required
for
the
solution
within
the
vessel
to
reach
the
maximum
purge
temperature.
The
vessel
was
placed
on
a
magnetic
stirrer
(
Ace
Glass,
Inc.,
No.
12064­
08),
and
a
1.
O­
in.
TFE
stirring
bar
agitated
the
solution.
Helium
was
directed
into
the
vessel
to
displace
the
headspace
at
40
mt/
min.
All
metal
gas
carrier
lines
beyond
the
vessel
outlet
were
wrapped
with
heat
tape
maintained
at
15OOC
to
prevent
condensation
of
the
target
analytes
and
internal
standards.
The
effluent
from
the
vessel
line
flowed
into
a
column
equipped
with
a
stopcock
and
frit
that
contained
1.0
mL
of
volatile­
free
water.
This
column
was
used
as
a
condenser
to
remove
excess
moisture
from
the
purge
gas.
The
outlet
line
from
this
purge
tower
was
attached
to
a
six­
way
Carle
valve.
A
GC
carrier
gas
line
of
helium
was
attached
to
the
Carle
valve.
The
Carle
valve
was
attached
to
a
glass­
lined
U­
tube
(
1/
8
i.
d.)
packed
with
a
1.0­
in.
plug
of
Tenax.
Glass
wool
was
used
to
maintain
the
position
of
the
Tenax
in
the
center
of
the
U­
tube.
The
U­
tube
was
rapidly
heated
(
within
5
to
8
s)
to
25OOC.
A
resistance
circuit
with
a
thermocouple
was
used
to
heat
and
regulate
the
Utube's
temperature.
In
the
purge
mode
the
Carle
valve
directed
the
purge
gas
and
analytes
into
the
U­
tube,
which
was
at
ambient
temperature.
The
analytes
were
trapped
and
the
purge
gas
vented.
The
helium
carrier
gas
was
directed
onto
the
HRGC
column
during
the
purge
mode.
After
the
purge
time
had
elapsed,
the
Carle
valve
was
switched
to
the
desorb
mode
and
the
U­
tube
was
heated
to
flash
volatilize
the
analytes.
The
helium
carrier
gas
was
then
routed
through
the
U­
tube
in
the
opposite
direction
of
the
purge
mode
and
directed
onto
the
HRGC
column.

2.
High
Resolution
Gas
Chromatography/
Mass
Spectrometry
The
volatile
organic
compounds
were
analyzed
using
a
finnigan
9610
GC
and
a
finnigan
4000
quadrupole
MS
equipped
with
an
INCOS
data
system.
Separation
of
the
volatile
organic
compounds
was
achieved
with
a
Durabond
DB­
5
fused
silica
capillary
column,
30
m
x
0.25
mm,
0.25­
pm
film
thickness
(
Jaw
Scientific,
Rancho
Cordova,
CA).
The
capillary
column
was
routed
directly
into
the
ion
source.
The
helium
carrier
gas
was
adjusted
at
12
psi
head
pressure
The
GC
was
equipped
with
a
Grob
type
split/
splitless
injector.
The
effluent
from
the
adsorbent
trap
was
adjusted
to
5
to
10
mL/
min
and
directed
8
Purse
Tower
with
Gioss
Frit
1Water
Ftow
Cmtr3l
fer
for
He
.

H20
in
Figure
1.
Schematic
of
apparatus
for
volati?
e.
organic
analysis.

9
000019
into
the
Grob
injector
with
a
syringe
needle
attached
to
the
stainless
steel
tubing
from
the
adsorbent
trap.
The
injector
was
operated
in
the
split
mode
with
a
1O:
l
split
ratio.

The
GC
was
held
isothermally
at
3OoC
for
5
min
and
then
programmed
at
6OC/
min
up
to
125OC
where
it
was
held
for
10
min.
Mass
spectral
data
were
acquired
across
the
mass
range
of
35­
275
amu
for
20
min
from
initiation
of
the
program.
The
HRGC
column
was
programmed
to
2OO0C
between
sample
analyses
as
a
precaution
to
ensure
that
all
materials
desorbed
from
the
Tenax
adsorbent
had
been
eluted
from
the
column
prior
to
the
next
analysis.

E
Analysis
Procedures
The
procedures
for
spiking
internal
quantitation
standards,
the
method
blank
analysis,
generation
of
calibration
curves,
and
composited
sample
analys
s
are
described
below.

1.
Spiking
Procedure
Internal
quantitation
standards
and
target
analytes
were
added
to
the
purge
tower,
method
blanks,
spiked
adipose
tissue
matrix
and
composite
samples
using
the
following
procedure.
A
35­
mm
length
of
TFE
tubing
was
inserted
over
the
needle
port
on
the
Leur
lock
assembly
of
a
10.0­
mL
syringe.
The
syringe
was
filled
with
3.0
mL
of
volatile
organic­
free
water
and
the
T,
FE
tubing
removed.
The
water
in
the
syringe
was
spiked
with
the
working
standards
(
using
a
5.0­
pL
syringe
and
needle)
through
the
needle
port,
and
the
TFE
tubing
was
replaced.
An
additional
2
mL
of
water
and
1.0
mL
of
air
was
then
drawn
into
the
10­
mL
syringe,
and
the
syringe
was
inverted
several
times
to
ensure
mixing
of
the
tetraglyme
and
water
solution.
The
contents
of
the
syringe
were
quantitatively
transferred
to
the
sample
vessel.
The
sample
vessel
was
tightly
capped
and
the
sample
was
allowed
to
sit
at
room
temperature
for
30
min
prior
to
initiating
the
analysis.

2.
Method
Blank
Analysis
The
Wheaton
vessel
was
filled
with
80
mL
of
the
volatile
organic­
free
water
and
spiked
with
1.0
pg
of
each
of
the
internal
quantitation
standards
The
vessel
was
quickly
capped
and
the
gas
flow
turned
on.
The
purge
tower
valve
was
kept­
in
the
off
position,
and
the
vessel
and
lines
were
leak
checked
with
vo?
atile
organic­
free
water.
Following
the
leak
check,
the
purge
tower
valve
was
opened,
the
hot
water
bath
valves
opened,
and
the
stirring
bar
turned
on.
The
headspace
above
the
stirred
mixture
was
purged
for
40
min
and
collected
on
the
Tenax
trap.

3.
Calibration
Curves
for
Reference
Standards
Calibration
curves
for
the
compounds
selected
as
reference
standards
were
developed
using
a
spiked
human
adipose
tissue
matrix.
The
spiked
adipose
tissue
matrix
is
referred
to
as
the
tissue
standard.
A
separate
20­
9
aliquot
of
a
bulk
adipose
matrix
was
used
to
prepare
each
tissue
standard.
These
tissue
standards
were
prepared
immediately
prior
to
analysis.
Preparation
of
the
spiked
tissue
samples
as
homogenize4
matrices
for
repeated
analysis
was
not
evaluated
in
this
study.

10
000020
.
.
,
,._
:.
T
'.
.
..:,<..
2
:,
:.

The
analysis
of
the
tissue
standard
was
performed
in'the
same
way
as
the
analysis
of
the
blank
but
with
20
g
of
human
adipose
tissue
added
to
the
Wheaton
vessel.
A
spatula
was
used
to
remove
the
frozen
tissue
from
the
sample
vials.
The
tissue
samples
were
spiked
with
1.0
pg
of
each
of
the
internaf
standards
and
0.2
to
1.4
pg
of
each
of
the
target
analytes.
Purge
time
was
40
min.

4.
Composi
ted
Sample
Analysis
The
composited
samples
were
analyzed
in
exact'ly
the
same
manner
as
the
tissue
standard
except
that
only
the
internal
standard
spiking
solution
wasxadded
to
the
aqueous
mixture.

F.
Quality
Control
Procedures
Figure
2
shows
the
general
volatire
organic
analysis
scheme
and
the
related
quality
control
(
QC)
procedures.
Daily
QC
procedures
included
the
analysis
of
reference
standards
and
internal
standards
spiked
in
the
purge
tower
(
instrument
performance
check);
a
system
blank
with
internal
standards;
a
reference
adipose
tissue
spiked
with
standards;
and
a
QC
sample.
The
QC
sample
consisted
of
either
an
additional
instrument
performance
check
to
verify
calibration
or
an
adipose'tissue
spiked
at
a
known
level
by
the
MS
analyst.
These
QC
samples
were
included
for
several
days
at
the
initiation
.
of
the
analysis
of
the
composites.
Also,
the
MRI
quality
control
coordinator
(
QCC)
periodically
submitted
blind
spikes
to
the
MS
analyst
to
assess
instrument
performance.
These
blind
spikes
were
added
to
the
purge
tower
before
proceeding
with
the
anlaysis.

The
results
of
these
analyses
are
provided
in
Section
V.
Before
proceeding
with
the
FY82
compositesspecimens,
the
MS
analyst
was
required
to
complete
successfully
the
analyses
of
check
samples
submitted
by
the
QCC.

G.
Data
Interpretation
The
HRGC/
MS
data
for
each
sample
were
interpreted
with
computer­
assisted
quantitation
routines.
A
mass
spectral
library
and
quantitation
list
of
the
target
analytes,
based
on
relative
retention
times
and
the
primary
characteristic
ion,
were
used
to
search
each
data
file.

1.
Qualitative
Identification
The
automated
search
quantitation
routine
identified
positive
re­.
sponses
based
on
the
primary
characteristic
ion
for
each
of
the
target
analytes
Table
l
provides
a
list
of
the
target
analytes,
primary
characteristic
quantitation
ions,
internal
standards,
and
the
relative
retention
times.
In
addition
to
the
automated
search,
the
MS
analyst
identified
compounds
by
reviewing
the
total
mass
spectra
at
the
specified
HRGC/
MS
scan
number.
This
effort
was
required
to
avoid
the
inclusion
of
false
positives
in
the
sample
set.
The
HRGC/
MS
data
were
also
reviewed
at
2
30
s
of
the
retention
time
of
each.
of
the
compounds
to
avoid
reporting
of
false
negatives.

13
f
Purge
Tower
Standard
1
I
*
Purge
Tower
QC
Internal
OC
Spike
­
Daity
Blind
OC
Spike
­
Weekly
Instrument
Performance
Eva
I
uation
Analytical
Method
Calibration
and
Evaluation
System
Blank
Spiked
Adipose
Tissue
Standard
(
20
g)
(
0.2
pg
­
1.4
pg)

Spiked
Adipose
Tissue
Sample
(
20
g)
lnterna?­
QC
Composlte
FY82
Adiwse
Tissue
Samples
(
5
­
20
g),

11
2
­
5
SampieslDay
I
1
i
t
Figure
2.
Analytical
scheme
for
analysis
of
volatile
organic
compounds
from
human
adipose
tissue.

12
000022
Table
1.
Characteristic
Ions,
Internal
Standards,
and
Relative
Retention
Times
Used
to
Identify
and
Quantitate
Target
Analytes
Primary
characteristic
quantitation
Target
analyte
ion
(
m/
z)

Bromochl
oropropane
Chloroform
d­
Chlor0form
l,
l,
l­
Trichloroehtane
Bromodichloromethane
Benzene
d,­
Benzene
fetrachloroethene
Dibromochloromethane
1,1,2­
Tri
chl
oroethane
To
1uene
d8­
Toluene
Chlorobenzene
ds­
Chl
orobenzene
Ethylbenzene
dlo­
fithylbenzene
Bromoform
5
tyrene
.
1,1,2,2­
Tetrach?
oroethane
d,­
l,
l,
2,2­
Tetrachl
oroethane
1,2­
Dichlorobenzene
d,
­
1
4­
Dich1orobenzene
1,4­
Dichlorobenzene
Xylene
dIo­
p­
Xylene
Ethylpheno1
77
79
82
97
129
78
a4
166
129
97
91
/

100
112
117
106
116
173'

104
83
84
146
150
146
106
116
122
­~

Internal
quakitation
standardb
RRT~

Bromochloropropane
1­
00
d­
Chl
oroform
0.20­
0.43
0.20­
0.43
Bromochl
oropropane
0.35­
0.58
Bromochloropropane
0.53­
0.76
ds­
Benzene
0.39­
0.62
0.39­
0.62
B
romoch1oropropane
1.16­
1.39
Bromoch1
oropropane
1.05­
1.2a
Brornochloropropane
0.88­
1.11
d8­
Toluene
0.83­
1.07
0.83­
1.07
d,­
Chl
orobenzene
1.48­
1.72
1­
48­
1.72
d,,­
Ethylbenzene
1.62­
1.85
1.62­
1.85
Bromochloropropane
1.79­
1.96
Bromochloropropane
1.85­
2.08
d2­
1,1,2,2­
Tetrachloroethane
2.05­
2.28
2.05­
2.
za
d4­
1,4­
Dich1orobenzene
2.88­
3.11
2.73­
2.96
d4­
1,4­
Dichlorobenzene
2.73­
2.96
d,,­
g­
Xylene
1.65­
1.88
1.65­
1­
88
dIo­
Ethylbenzene
2.19­
2.43
aRelative
retention
times
calculated
versus
the
internal
want
tat
on
standard,
bbromochloropropane.
Designation
indicates
the
pairing
of
the
target
analytes
with
the
respective
internal
standards.

13
000023
2.
Quantitation
Data
were
quantitated
based
on
either
the
internal
standard
or
the
isotope
dilution
principle.
The
isotope
dilution
principle
applies
to
the
quantitation
of
target
analytes
for
which
a
deuterated
analog
was
available
as
an
internal
standard.
Where
possible,
the
deuterated
analog
of
a
target
analyte
was
used
for
quantitation.
Other
compounds'
concentrations
were
cal
culated
versus
the
internal
standard,
brornochloropropane
(
1­
chloro­
2­
bromo
propane).

The
HRGC/
MS
data
were
quantitated
using
the
following
equation:

A,
x
IS
3
Target
analyte,
1.19=
AIS
x
RRF
where
As
=
area
of
the
characteristic
quantitation
ion
of
the
target
analyte,

=
area
of
the
characteristic
quantitation
ion
of
the
internal
standard,

IS
=
amount
of
the
internal
standard
in
micrograms
(
pg),

RRF
=
relative
response
factor
of
the
target
analyte
versus
the
respective
internal
standard
The
concentration
(
vg/
g)
of
the
target
analyte
in
the
original
sample
was
calculated
by
dividing
the
total
micrograms
of
target
analyte
detected
by
the
composite
weight.
In
this
report
concentration
data
are
expressed
in
either
micrograms
per
gram
(
pg/
g)
or
nanograms
per
grain
(
ng/
g).

The
quantitative
data
were
qualified
based
on
the
observed
response
for
each
target
analyte
and
the
corresponding
internal
standard.
Compounds
for
which
no
positive
response
was
observed
are
reported
as
not
detected
(
ND).

,
An
estimated
limit
of
detection
(
LOD)
was
calculated
based
on
the
observed
instrumental
response
for
the
specific
target
analyte
and
corresponding
internal
standard.
in
each
sample.
The
LOD
was
estimated
as
the
amount
of
a
specific
analyte
that
must
be
present
to
give
rise
to
a
signal
at
least
2.5
times
the
background
signal­
to­
noise.

Compounds
detected
for
which
the
observed
response
of
the
characteristic
quantitation
ion
was
greater
than
2.5
times
but
less
than
10
times
the
background
signal­
to­
noise
are
reported
as
trace
(
tr)
values.
Target
analytes
detected
at
greater
than
10
times
the
background
signal­
to­
noise,
limit
of
quantitation
(
LDQ),
are
reported
as
positive
quantifiable
values.

All
data
were
corrected
for
blank
values
observed
for
the
system
blank
run
daily
with
each
set
of
samples.

H.
Method
Validation
The
analytical
method
was
evaluated
by
analyzing
adipose
tissue
specimens
fortified
with
known
levels
of
specific
volatile
organic
compounds.

14
000024
I
..

These
experiments
were
designed
to
evaluate
the
use
of
the
internal
standards
recommended
for
 PA
Method
624
(
USEPA
1984)
for
determination
of
volatile
organics
in
water
and
wastewater
(
bromochloromethane,
bromochloropropane,
and
1,4­
dichlorobutane),
as
well
as
multiple
deuterated
analogs
of
specific
target
analytes
(
isotope
dilution).
Preliminary
studies
demonstrated
that
the
internal
standards,
bromochloromethane
and
1,4­
dichlorobutane,
were
not
adequately
recovered
from
the
adipose
tissue/
water
mixtures.
Bromochloropropane
provided
reasonable
response
from
the
spiked
adipose
matrix
and
was
further
evaluated
as
a
quantitation
standard.

The
results
of
the
analysis
of
adipose
tissue
spiked
with
nine
volatile
compounds
at
four
concentration
levels
ranging
from
5
to
75
ng/
g
(
ppb)
are
presented
in
Table
2.
In
general,
the
average
recovery
of
the
analyses
for
these
compounds
was
good,
except
for
chloroform,
which
demonstrated
an
average
recovery
of
264%.
Although
the
average
recovery
for
the
other
compounds
was
quite
good
(
62
to
116%),
wide
variability
was
noted
for
the
individual
analyses
at
each
spike
level.

The
high
recovery
of
chloroform
from
this
study
may
be
a
result
of
a
difference
in
the
background
chloroform
concentration
in
the
adipose
tissue
used
for
this
spiking
experiment
as
compared
to
the
tissue
used
for
calibration.
An
absolute
value
for
the
background
contribution
of
each
target
analyte
was
not
determined
from
unspiked
tissued
used
in
these
experiments­
Another
factor
that
may
have
resulted
in
the
high
recovery
of
chloroform
is
the
possible
conversion
of
trichloroacetic
acid
(
present
as
a
metabolite
of
tetrachlroethylene,
trichloroethane,
etc.).
to
chloroform
at
the
elevated
temperatures
required
to
complete
the
analyses
(
Peoples,
Pfaffenberger,
Shafik,
Enos
1979).

The
impact
of
the
use
of
multiple
internal
standards
versus
a
single
internal
standard
was
evaluated
as
a
separate
experiment.
Deuterated
analogs
of
several
target
analytes
were
added
to
fortified
tissue
samples
in
addition
to
bromochloropropane,
Table
3
presents
the
comparison
of
the
single
versus
multiple
internal
standard
quantitation
techniques.
As
noted
in
Table
3,
a
deuterated
analog
was
not
available
for
tetrachloroethene.
The
data
generated
for
the
target
analytes
demonstrate
average
recoveries
ranging
from
82
to
136%
for
the
multiple
internal
standard
quantitation
as
compared
to
average
recoveries
of
74
to
143%
for
the
same
compounds
quantitated
versus
bromochloropropane.
The
somewhat
tighter
range
of
recoveries
or
accuracies
of
quantitation
with
incorporation
of
the
multiple
internal
standards
results
from
the
fact
that
the
deuterated
ana logs
behave
similarly
to
the
target
analytes.

The
purging
efficiencies
of
the
target
analytes
and
the
internal
standards
were
evaluated
from
replicate
analyses
of
a
single
fortified
adipose
tiss6e.
This
experiment
was
necessary
to
(
1)
demonstrate.
the
difference
in
partitioning
of
the
various
target
anafytes
from
the
water/
tissue
mixture
to
the
headspace
and
(
2)
compare
the
partitioning
characteristics
of
the
available
internal
standards
versus
the
target
analytes.
A
20­
9
aliquot
of
tissue
was
spiked
with
1.0
yg
each
of
the
internal
standards
and
0.20
pg
of
the
target
analytes.
The
sample
was
heated
to
approximately
8OoC,
and
the
headspace
above
the
stirred
mixture
was
sampled
for
40
min.
The
volatile
compounds
were
desorbed
from
the
Tenax
adsorbent
and
analyzed
by
HRGWMS.
The
heating,
purging
sampling,
and
analysis
procedures
were
repeated
an
additional
three
times.

15
a3
L
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.
a
1=
r
S
+
J
c,
aJ
Q,
aJ
a
W
N
1­­
0
0
c
0
c
Q,
L
aJ
n
c
­
0
N
0
a
I­
m
3
c
c
00
P
W
t
.
t=
L
E
S
U
­
n
U
0
a
m
7
u
0
­
3
L
A
L
c
c1
.
c
c,
0
a,
&
W
'?
U
I
I­
I
I­
w
#­­
13
a
17
The
absolute
area
counts
for
the
characteristic
quantitation
ion
for
each
com
pound
were
recorded.
The
data
for
each
compound
monitored
are
provided
in
Figures
3
to
6
and
are
plotted
as
absolute
area
counts
versus
the
sample
run
number.

Figure
3
is
a
plot
of
the
three
internal
standards
used
in
EPA
Method
624
for
volatiles
in
water
and
wastewater.
Three
distinctive
plots
for
the
three
internal
standards
are
presented.
These
data
demonstrate
that
bromochloromethane
is
not
an
acceptable
internal
standard
due
to
low
response.
The
breakthrough
volume
for
the
volatile
components
is
based
on
the
total
sample
volume
mass
of
adsorbent
and
sampling
temperature.
Based
on
sampling
volumes
extrapolated
by
Brown
and
Purnell
(
19771,
it
is
expected
that
the
optimum
sampling
volume
for
the
more
volatile
components,
such
as
bromochloromethane
are
approximately
9
to
10
L
per
gram
of
Tenax
adsorbed.
The
total
sample
volume
used
in
these
experiments
was
1.6
L
(
40
mL/
min
for
40
min)
and
the
total
mass
of
Tenax
was
approximately
0.2
g.
Hence,
the
low
response
observed
for
bromochloromethane
is
probably
due
to
the
low
capacity
of
the
Tenax
adsortjent
system
for
the
more
volatile
compounds
rather
than
to
the
purging
efficiency
from
the
matrix.

The
plot
of
bromochloropropane
indicates
that
this
internal
standard
is
effectively
partitioned
from
the
adipose/
water
mixture
to
air
for
all
four
analyses.
The
plot
for
1,4­
dichlorobutane,
on
the
other
hand,
indicates
that
this
compound
is
fairly
soluble
in
the
adipose/
water
matrix.
The
adipose/
air
partitioning
constant
is
obviously
low.
Hence,
this
compound
was
not
considered
as
a
quantitative
internal
standard
for
further
sample
analyses.

Figure
4
presents
additional
plots
of
the
observed
purging
efficiencies
for
eight
deuterated
internal
standards
spiked
initially
at
1.0
pg
in
the
20­
9
adipose
tissue
sample.
Again
it
is
noted
that
the
deuterated
analog
of
chloroform
was
detected
only
in
the
first
sample
analysis.
This
observation
is
possibly
due
to
the
fact
that
chloroform
has
the
lowest
boiling
point
(
b.
p.
6O.
5­
61,
S0C),
hence
greatest
volatility,
of
the
compounds
analyzed.
Deuterated
methylene
chloride
(
d,­
CH2C12)
was
also
added
to
these
samples
but
was
not
detected
even
in
the
first
analyses.
The
plots
of
the
other
internal
standards
appear
to
reflect
the
effect
of
boiling
point
on
purging
efficiency
from
the
heated
mixture.
The
d6­
benzene
and
d,­
toluene
demonstrate
the
most
significant
differences
in
absolute
response
for
the
sequential
analysis
of
the
spiked
adipose
sample.
The
boiling
points
for
these
compounds
range
from
approximately
80
to
lll
°
C
as
compared
to
135
to
173OC
for
d,,­
R­
xylene
and
d4­
l,
4­
dichlorobenzene.

The
absolute
responses
of
several
target
analytes
spiked
(
0.20
pg
each)
into
the
same
20­
9
aliquot
of
human
adipose
are
plotted
for
the
four
sequential
analyses
(
Figures
5
and
6).
The
plots
for
these
target
analytes
also
appear
to
correspond
with
the
boiling
points
of
the
specific
compound.
The
more
volatile
cempounds
such
as
chloroform
(
b.
p.
60.5­
61.
S"
C),
l,
I,
l­
trichloroethane
(
b.
p.
74­
76OC),
and
dibrornochloromethane
(
b.
p.
119­
12OoC)
were
detected
in
only
the
first
and
second
analyses,
indicating
better
purging
efficiency
a1though
less
retention
on
the
Tenax
adsorbent,
than
demonstrated
for
the
other
compounds.
The
response
profiles
noted
for
compounds
such
as
benzene,
toluene,
chlorobenzene,
tetrachloroethene,
ethylbenzene,
and
dichlorobenzene
are
very
similar
to
the
plots
of
the
deuterated
analogs
presented
in
Figure
4.

18
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..

Q)
C
0
a
a,
OSwv
h
EU
0
Lrn
+.
I=
.

1P
0
­
w
m
~

c,
L
Y­
13
i
00
19
c
m
E
3
c
uwE5
3
20
st.
a
0
0
0
*
0
0A
000031
0'
v
22
P
.
C
c
*­
L
Q7
ma
040
nn
urn
f
C
3
er:

XL.­
3
­
0
4le
OL
22
000032
I
,­
I
The
similarity
in
the
response
profiles
for
several
target
analytes
and
the
corresponding
deuterated
analogs
are
presented
in
Figures
7
to
9.
These
plots
reflect
that
the
purging
efficiencies
of
each
pair
of
compounds
are
equivalent
from
the
spiked
adipose
tissue.
These
plots
demonstrate
the
advantages
of
the
isotope
dilution
(
target
analyte/
deuterated
internal
standard
pair)
technique
versus
a
single
internal
standard
for
quantitation
of
volatile
organics
in
human
adipose
tissue.
With
the
exception
of
toluene,
the
differences
of
responses
noted
for
these
pairs
are
roughly
a
factor
of
5
for
each
analysis,.
which
corresponds
to
the
spike
ratio
of
0.20
pg
of
target
analyte
versus
1.0
pg
for
the
deuterated
internal
standard.
The
difference
noted
for
the
toluene/
d8­
toluene
plot
is
the
result
of
the
endogenous
toluene
concentration
in
the
tissue
sample
used
for
these
analyses.

Figure
10
provides
a
plot
of
the
obse.
rved
responses
for
several
com
pounds
not
spiked
into
the
tissue
sample.
These
compounds
include
1,4­
dichlo
robenzene,
two
xylene
isomers,
and
three
C3­
alkyl
benzenes
(
trimethyl,
methyl­
ethyl,
or
propyl
isomers).
These
results
indicate
that
the.
method
might
be
capable
of
detecting
and
quantitating
compounds
with
boiling
points
ranging
up
to
approximately
175OC.

IV.
RESULTS
The
analyses
for
the
NHATS
FY82
composite
samples
were
completed
following
the
method
evaluation
studies.
Figures
11
to
17
provide
examples
of
the
HRGC/
MS
chromatograms
for
the
analysis
of
instrument
performance
checks,
spiked
tissue
samples,
and
actual
composite
samples.

Figures
12
and
13
compare
the
HRGC/
MS
chromatogram
of
the
bulk­
adipose
tissue
used
to
establish
method
performance
and
one
of
the
composite
samples.
The
HRGC/
MS
chromatogram
of
the
composite
sample
appears
to
have
considerably
more
volatile
material
than
the
bulk
adipose
used
to
prepare
the
tissue
standard.
Tentative
identifications
for
some
of
the
major
peaks
in
Figure
13
were
assigned
based
on
the
comparison
of
the
mass
spectra
to
library
spectra.

figures
14
and
15
provide
comparisons
of
the
composite
specimens
for
three
age
groups
within
the
same
census
division.
All
of
the
samples
from
each
census
division
were
analyzed
on
the
same
day.
The
results
demonstrate
that
the
elution
profiles
of
all
samples
are
comparable
although
the
absolute
responses
of
the
peaks
vary.

Figures
16
and
17
provide
comparisons
of
three
composite
samples
representing
the
15­
44and
0­
14age
groups
from
three
census
divisions.
Again
the
general
HRGC/
MS
profiles
appear
to
be
consistent
although
the
absolute
response
of
each
peak
varies
from
sample
to
sample.

23
cp
0
­.
a
C
m
­
5
aJ
CJ
m
L
ii
m
80
000034
D"

­,

..
v)
L
S8­
l
80
I
0­
r4
o­­

It
0
ao
B
s
z
C
PL
N
v
­

000035
m
.
a
.
I.

/

26
*
W
'
C
0,
N
c
a2
5
I
hc
U
a
E
3
r
0
4.
cmou40.

0
I­
7
f
c
v)
3
Yoc
OL
U
3
A0
.

ILL
27
000037
.

1.
Benzene/
dg­
benzene
2.
3romodichloromethane~
3.
Toluene/
d8­
toluene
4.
Bromochloropropane/
1,
l
,
Z­
trichJoroethane
5.
DibromochI
orometha
ne
6.
Tetrachloroethene
7.
Chlorobenzene/
dg­
chlorobenzene
8.
d10­
ethy1benzene
9.
Ethylbentene
10.
dlo­
p­
xylene
11,
8romoform
12.
Styrene
13.
Dichlorobutone
14.
1,1,2,2­
tetrachloroethane
15.
d4­
1,4­
dichIorobenzene
16.
1,2­
dichlorobenzene
Purge
Tower
5tandard
14
r
16
I
i
*
lor80
Fiqure
11.
HRGC/
MS
chromatoqram
of
purge
tower
standard
analyzed
daily
to
document
instrument
performance.

28
1
.
Chioroform/
d­
chloroform
2,
Bromochtororqethane
3.
1,
I,
I­
trichloroethane
4.
BenzeneJdg­
benzene
5.
Bromodichloromethane
6.
Toluene/
dg­
to
1uene
7.
1,
?
,2­
trichloroethane
8.
Di
bromoch1
oromethane
9.
Tetroch
Ioroethene
.
10.
Chlorobenzene/
.
dg­
ch
1
orobenzene
11.
dl0­
ethylbentene
12,
Ethylbenrene
13.
dl~­
p­
xyJene
14.
Bromoform
15.
Styrene
16.
1,1,2,2­
tetrachloroethane/
d2­
lf1,2,2­
tetrachloroethane
17.
d4­?
,4­
dic
h
lorobentene
18.
1,2­
dichlorobenzene
Tissue
Standard
lee.

BfE
3I2e
.
&
e
.
.

Figure
12.
HRGC/
MS
chromatogram
for
the
volatile
organic
analysis
of
a
bulk
adipose
(
tissue
standard)
spiked
with
1.0
pg
of
each
internal
standard
and
0.20
pg
of
each
target
analyte.

29
'

000039
Tentative
Identification
of
Major
Peaks
1.
Acetic
acid
ethyl
ester/
Propanoic
acid
propyl
ester
2.
Heptanal
3.
Decane
4.
Dimethyfoctane
5.
Trimethylcycfohexane
6.
Nonanal
7.
Undecene
8.
Ethyl
ester,
carboxylic
acid
9.
Nonadienul
Middie
Atlantic,
0­
14
years
5
7
Figure
13.
HRGC/
MS
chromatogram
of
volatile
compounds
from
the
NHATS
FY82
composite
of
the
0­
14
year
age
group
from
.
the
Middle
Atlantic
census
division.

30
080040
Middle
Atlantic
45
plus
years
Middle
Atlantic
15­
44
years
Middle
Atlantic
0­
14
years
Figure
14.
Comparison
of
the
HRGC/
MS
chromatograms'for
the
volatile
organic
analytes
for
three
composite
age
groups
from
the
Middle
Atlantic
census
division.
31
000041
East
North
Central
45
plus
years
East
North
Central
15­
44
years
.

East
North
Central
0­
14
years
,
1llY
Figure
15.
Comparison
of
the
HRGC/
MS
chromatograms
for
the
volatile
organic
analytes
for
three
composite
age
groups
from
the
East
North
Central
census
division.
32
000042
Middle
Atlantic
15­
44
years
East
North
Central
15­
44
years
West
North
Centrai
15­
44
years
.
Figure
16.
Comparison
of
the
HRGC/
MS
chromatograms
of
the
volatile
organic
analysis
of
three
composite
specimens
representing
the
15­
44
age
group
from
three
census
divisions.
33
000043
Middle
Atlantic
0­
14
years
LJ
rt
7
East
North
Central
0­
14
years
West
North
Centra1
0­
14
years
.
Figure
17.
Comparjson
of
the
HRGC/
MS
chromatograms
of
the
volatile
organic
analysis
of
three
composite
specimens
representing
the
0­
14
age
group
from
three
census
divisions.
34
000044
Seventeen
target
analytes
were
determined
using
the
automated
HRGC/
MS
search
routines
and
the
mass
spectral
library
established
in
the
method
evaluation
studies.
Figures
18
to
21
summarize
the
incidence
of
detection
of
each
of
these
analytes
by
age
and
by
census
division
within
the
four
regions.
A
plus
indicates
that
the
compound
was
detected
in
the
analysis
of
a
particular
composite.
A
minus
indicates
the
compound
was
not
detected
above
the
estimated
limit
of
detection.
The
number
of
symbols
shown
under
each
age
category
for
a
specific
compound
indicates
the
total
number
of
composi
tes
analyzed.
.
The
quantitative
data
for
the
17
target
analytes
are
shown
in
Tables
4
through
20
b)
census
division
and
age
group.
The
tables
provide
the
total
wet
tissue
weight
composited,
the
total
mass
of
the
specific
analyte
detected,
the
concentration
based
on
the
original
wet
tissue
weight,
and
the
analysis
date.
The
tables
provide
estimated
limits
of
detection
for
composites
for
which
a
compound
was
not
detected
(
ND)
and
for
composites
for
which
the
compound
is
reported
as
a
trace
(
tr)
value.
Trace
values
are
reported
for.
responses
observed
at
greater
than
2.5
times
the
signal­
to­
noise
but
less
than
10
times
signal­
to­
noise.
Data
reported
with
no
qualifier
indicate
a
positive
response
detected
above
the
limit
of
quantitation
(
LOQ)
or
greater
than
10
times
the
background
signal­
to­
noise.

Upon
reviewing
the
data
in
Tables
4
through
20
reported
as
not
detected
(
ND),
it
is
noted
that
the
level
of
detection
(
total
micrograms)­
varies
from
one
sample
to
another.
This
results
from
a
combination
of
the
observed
background
in
a
sample
at
the
characteristic
ion
for
a
specific
analyte
and
the
intensity
of
the
response
of
the
characteristic
ion
for
the
corresponding
internal
standards.
Hence,
the
calculated
limits
of
detection
were
higher
in
some
instances
due
to
high
background
at
the
charasteric
ions
for
the
target
analytes
and/
or
low
recovery
(
observed
as
intensity
of
repsonse)
of
the
associated
internal
standards.

4.
Table
21
presents
the
frequency
of
observation
of
the
target
analytes
from
the
46
composite
samples.
Styrene,
1,4­
dichlorobenzene,
xylene
isomers,
and
ethylphenol
were
detected
in
all
46
composites.
Two
responses
were
observed
that
correspondedLto
xylene
isomers.
However,
the
isomers
are
not
specified
since
the
order
of
elution
of
the
three
possible
compounds
was
not
determined.
Benzene,
chlorobenzene,
ethylbenzene,
and
toluene
were
detected
in
nearly
all
composites.
Tetrachloroethane,
1,2­
dichlorobenzene,
and
l,
l,
l­
trichloroethane
were
detected
in
approximately
50
to
60%
of
all
composite
specimens.
1,1,2,2­
Tetrachloroethane
was
detected
in
less
than
10%
of
all
composite
samples
(
4
of
the
46).
The
three
brominated
target
analytes
and
L,
l,
2­
trichloroethane
were
not
detected
in
any
of
the
composite
specimens.

The
quantitative
data
for
all
compounds
detected
in
a
specific
com
posite
are
reported
in
Tables
B­
l
to
B­
18
in
Appendix
B.

35
­­
­­
­­
­­

­­
­­
­­

­­
­­
­­

­­
­­
­­
Census
Region
Census
division:
Age
group:

Compound
Northeast
New
England
Middle
Atlantic
0­
14
15­
44
45+
0­
14
15­
44
45+

Chloroform
+
+
+
+­++
++

1,
l,
l­
Trichloroethane
­
+
­++

Bromodi
chloromethane
Benzene
++
++

Tetrachloroethene
­­­++
++
++

­­­
Dibromochloromethane
l,
l,
2­
Trichloroethane
,
­­­­­­­­­

Toluene
+
+
+
++
++
++

Chlorobenzene'
.
'
+
+
+
++
++
++

Ethylbenzene
+
+
+
++
++
++

­­
Bromoform
e
+
+
+
++

­

+
+
++
++
++.

++
++
Styrene
1,1,2,2­
Tetfachloroethane
1,2­
Dichlo.
robenzene
.
1,4­
Dichlorobenzene
+
+
+
++
++
++

X~
I
enea
+
+
+
++
++
.
++

Ethylphenol
+
+
+
++
++
++

afhe
exact
i
somers
were
not
determined.

Figure
18.
Incidence
of
detection
of
volatile
organic
compounds
in
composited
human
adipose
tissues
from
the
Northeast
census
region.
The
total
number
of
+
and
­
symbols
for
a
specific
compound
indicates
the
number
of
composites
analyzed
for
each
age
group.

36
­­

­­
­­
­­

­­

­­
­­­­

­­­­

­­­­
­­

­­
­­

­­
­­

­­

­­
Census
Region
Census
division:
Age
group:

ComQound
Chloroform
1.1
,
l­
Trichloroethane.

Bromodichloromethane
Benzene
Tetrachl
oroethene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
l,
l,
Z,
Z­
Tetrachloroethane
1,2­
Dichlorobenzene
1,4­
Dithlorobenzene
X~
I
mea
Ethyl
phenol
a 
The
exact
isomers
were
not
determined.
South
Atlantic
0­
14
15­
44
45+

++
+++

+++

++++

++++

­­­..

+­++++

++
*+++

++
++++

++
++++

­..­

­+­

++++

++
++++

++
++++
South
­
East
South
Central
West
South
Cent
0­
14
15­
44
45+
0­
14
15­
44
­+
++

­+
­+

++
++

++
­+

..
c
++
­+

++
++

++
++
..

++
++
.

­+
+

+

++

++
++.

++
++

Figure
19.
Incidence
of
detection
of
volatile
organic
compounds
in
composited
human
adipose
tissues
from
the
South
census
region.
The
total
number
of
+
and
­
symbols
for
a
specific
compound
indicates
the
number
of
composites
analyzed
for
each
age
group.

37
000047
­­
­­

­­
­­

­­

­­
­­

­­­

­­­
­­­

­­­
­­­

­­­

­­­
­­

­­
­­

­­

­­
*.
.

~­

Census
Region
Census
division:
Age
group:

Compound
Chloroform
l,
l,
l­
Trich?
oroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Dibromochloromethane
1,1,2­
Trichloroethane
To7uene
Chlorobenzene
Ethyl
benzene
i3romoform
Styrene
Northcentral
East
North
Central
West
North
Central
0­
14
15­
44
45+
0­
14
15­
44
45+

++
+++
+++
+

­+­­­+
­+

++
+++
++­++

+­­++
­++
+*

++
+++
+++
++

++
+++
+++
++

++
+++
+++
++

++
+++
+++
++

l,
l,
Z,
Z­
Tetrachloroethane
+­

1,2
Dichlorobenzene
.
++
++­+­+
+­

1,4­
Dichlorobenzene
++
++
f
+++
++

xyl
enea
++
++
f
+++
++

Ethy1pheno1
++
+++
+++
++

­~~
a
The
exact
isomers
were
not
determined.

Figure
20.
Incidence
of
detection
of
volatile
organic
compounds
in
composited
human
adipose
tissues
from
the
North
Central
census
region.
The
total
number
of
+
and
­
symbols
for
a
specific
compound
indicates
the
number
of
composites
analyzed
for
each
age
group.

38
Census
Region
­
Census
division:
Mountain
Pacific
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+
Compound
Chloroform
+
+
+
+
+
+
West
1,1,
l­
Tri
chloroethane
­+
+
+
+

Benzene
4.
+
.+
+
+.
+
­­­
Tetrach1
oroethene
+
4.
+
­­­­
Dibromochl
oromethane
­­
­­­
l,
l,
Z­
Trichloroethane
­'
*
­

To
1
uene
+
+
+
+.
+
+

Chlorobenzene
+
­
5­+
+
+
+

Ethylbenzene
­+
+
+
+
+
+
­­­­­­
5romoform
Styrene
+
i
+
­
i
+
+'
­­­­­
l,
l,
Z,
Z­
Tetrachloroethane
,
­

1,2­
Dich1
orobenzene
*
­+
+
+
+
+

1,4­
Dichlorobenzene
+
+
i
+
+
i
eneaxy~
+
+
+
+
+
+

Ethyl
pheno1
+
+
+
+
+
+

,
I
aThe
exact
isomers
were
not
determined.

Figure
21­
Incidence
of
detection
of
volatile
organic
compounds
in
composited
human
adipose
tissues
from
the
West
census
region.
The
total
number
of
+
and
­
symbols
for
a
specific
compound
indicates
the
number
of
composites
analyzed
for
each
age
group,

39
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000083
Table
21.
Incidence
of
Detection
of
Selected
Volatile
Organic
Compounds
in
the
NHATS
FY82
Composite
Samples
Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Dibromochloromethane
1,1,
P­
Trichloroethane
To1uene
Ch7orobeniene
Ethy1
benzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1,4­
Dichlorobenzene
Xylene
Ethylphenol
Frequency
of
observation
(%)

76
48
0
96
61
0
0
91
96
96
0
100
9
63
100
100
100
74
000084
V.
QUALITY
ASSURANCE/
QUALITY
CONTROL
As
mentioned
in
Section
IV,
several
procedures
were
included
with
the
analysis
of
the
composite
specimens
to
document
the
quality
of
the
data
reported.
These
procedures
included
instrument
performance
checks
using
re
agent
spikes
at
the
purge
tower.
These
were
performed
daily
following
initial
instrument
cal
ibration
by
the
HRGC/
MS
analyst.
The
quality
control
procedures
also
required
that
the
analyst
demonstrate
background
contribution
of
the
headspace
analysis
system
through
the
analysis
of
system
blanks.
Adipose
tis
sue
samples
were
spiked
with
known
amounts
of
the
target
analytes
and
internal
standards
to
verify
consistency
of
response
factors
before
proceeding
with
the
sample
analyses.
When
necessary,
the
analyst
completed
the
analysis
of
a
three­
point
calibration
curve
before
proceeding
with
sample
analysis.
Typical
.
spike
levels
of
the
target
analyte
ranged
from
0.2
to
1.4
1.19per
20­
g
aliquot
of
tissue.
These
spike.
levels
were
equivalent
to
concentrations
from
0.010
to
0.070
pg/
g.

A.
Instrument
Performance
Checks
Instrument
performance
checks
were
completed
using
quality
control
samples
prepared
by
the
MS
analyst
(
internal
QC)
or
by
the
project
quality
control
coordinator
(
external
QC).
These
instrument
performance
checks
were
completed
to
demonstrate
that
the
HRGC/
MS
system
was
properly
calibrated
and
to
document
method
performance
(
precision)
over
time.
The
instrument
performance
checks
were
achieved
by
spiking
a
solution
of
the
reference
compounds
into
the
purge
tower
and
then
proceeding
with
the
sampling
and
analyses
events
as
described
earlier
in
the
experimental
section.

1.
Internal
QC
Table
22
presents
a
summary
of
the
internal
QC
instrumental
performance
check
completed
for
10
different
analysis
days.
Spike
levels
for
these
instrument
performance
checks
were
from
0.20
to
0.40
pg
for
each
of
the
specified
target
analytes.
Table
23
provides
the
average
recovery
and
range
of
measured
recoveries
for
each
compound.
As
noted,
the
method
recoveries
for
 
all
compounds
were
typically
within
the
range
of
80
to
120%
with
the
exception
of
bromochloromethane.
The
method
precision
for
the
internal
QC
measurements
was
generally
within
f
15%.
These
accuracy
and
precision
estimates
reflect
day­
to­
day
performance
of
the
analytical
method.

2.
External
QC
A
mixed
volatile
stock
standard
was
prepared
containing
chloroform,
benzene,
bromodichloromethane,
toluene,
chlorobenzene,
ethylbenzene,
1,
Z­
dichlorobenzene
1,1,2,2­
tetrachloroethane,
and
tetrachloroethene
at
a
concentration
of
10
mg/
mL
for
each
compound.
One
portion
of
the
stock
solution
was
diluted
and
used
for
internal
QC,
and
another
was
diluted
and
used
for
performance
audit
samples.

Five
dilutions
of
the
stock
solution
were
prepared
in
tetraglyme,
sealed
in
microreaction
vials
sealed
with
Mininert
valves,
and
stored
in
a
freezer
until
needed.
The
concentration
of
each
compound
per
dilution
was:

75
Audit
sample
no.
VOA
1
VOA
2
VOA
3
VOA
4
VOA
5
Concintration
0.41
pg/
pL
0.80
pg/
pL
0.80
pg/
pL
0.68
crn/
uL
0.81
&
bL
The
results
of
the
QC
performance
audit
samples
are
founG
in
Table
24.

B.
Spiked
Adipose
Tissue
Samples
An
additional
QC
control
check
included
the
analysSs
of
spiked
adipose
tissue
samples.
Table
25
summarizes
the
results
for
five
spiked
adipose
tissue
specimens
analyzed
with
the
first
sample
batches.
The
mean
accuracy
of
these
measurements
ranged
from
94%
for
l,
l,
Z­
trichloroethane
to
14%
for
1,1,2,2­
tetrachloroethane.
The
range
of
recoveries
for
each
compound
is
somewhat
broader
than
noted
for
the
instrument
performance
checks
due
to
the
influence
of
the
matrix
on
recovery
efficiency
and
background
contribution.

C.
Internal
Standards
The
absolute
responses
of
the
internal
standards
were
noted
for
each
QC
check
sample
and
composite
adipose
tissue
sample
to
document
instrument
operating
parameters.
The
absolute
responses
of
the
internal
standards
in
the
first
composite
sample
analyzed
were
observed
to
decrease
markedly
in
comparison
to
the
responses
observed
for
the
instrument
performance
check
and
system
blank.
A
reduction
in
the
response
can
be
attributed
to
the
adipose
Obviously,
the
presence
of
oily
lipid
materials
affects
the
tissue
matrix.
aqueous
to
air
partitioning
of
the
volatile
internal
standards.

Differences
in
the
recovery
of
the
internal
standard
from
the
FY82
composite
specimens
and
the
bulk
adipose
tissues
used
for
method
calibration
were
also
observed.
The
absolute
responses
of
the
internal
standards
from
the
bulk
adipdse
tissue
samples
were
nearly
always
greater
than
the
responses
for
the
NHATS
composites.
This
indicates
that
the
recoveries
or
observed
partitioning
of
the
.
internal
standards
from
the
spiked
samples
to
the
headspace
was
greater
for
the
QC
samples
than
the
FY82
composites.
This
observed
recovery
might
indicate
some
difference
in
the
two
sources
of
adipose
tissues.
This
bulk
adipose
tissue
had
been
collected
within
6
mo
of
the
volatile
organic
analysis
as
compared
with
the
FY82
specimens,
which
had
been
stored
for
up
to
2
yr.

After
observing
the
reduction
in
response
with
the
first
composite
sample,
the
instrument
performance
was
verified
through
reanalysis
of
a
vessel
blank
(
water
plus
internal
standards).
This
analysis
demonstrated
that
the
instrument
was
properly
calibrated
and
that
the
matrix
was
responsible
for
the
reduction
in
response
of
the
internal
standards.

Figures
22
to
25
are
plots
of
several
of
the
internal
standard
responses
from
the
system
blanks,
spiked
reference
tissue
samples,
and
NHATS
composite
samples.
These
plots
demonstrate
that
the
differences
in
the
observed
internal
standards
responses
for.
the
method
blanks,
spiked
reference
tissues,
and
the
NHATS
composites
were
noted
for
each
day
that
the
composites
were
analyzed.

76
000086
w
*
Q~
uOOmONOOdd
n
mmor?
wmmoo~
ww
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ln
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77
000087
fable
23.
Average
Recovery
for
Intsrnal
QC
Instrument
Performance
Checks
Compound
Average
recovery
(%)
Range
(%)

l,
l,
l­
Trichloroethane
Bromochloromethane
105
2
11.8
121
k
71
90­
125
50­
280
Benzene
98.3
It
4.9
90­
105
Tetrachloroethene
99.3
k
8.9
88­
115
Dibromochloromethane
98.8
f
6.1
90­
110
1,1,2­
Trichloroethane
.
To1uene
101
f
5:
7
103
2
12.1
90­
110
88­
120
Chlorobenzene
103
k
6.7
95­
120
Ethylbenzene
Bromoform
100
+,
5.3
99.5
k
12.3
90­
110
80­
115
Styrene
l,
I,
Z,
Z­
Tetrachloroethane
1,2­
Dichlorobenzene
103
rt
14.6
101
k
9.4
102
k
7.9
90­
140
80­
110
90­
115
.
aThese
data
were
summarized
to
include
accuracy
for
isotope
dilution
measurements
where
possible.

78
000088
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0
cu
r(
rl
­
4
OD
0
0
03
3
I4
0,
00
d
0)

I:
rl
rl
I
V
rl
0
0
F­
0
0
o',
ps
*
rl
4
NON
u
d
N
.­
I
N
c\
I
r)
l­
4
N
6
N
N
N
3
0
0
0
0
0
0
0
0
0
4
0
0
0
.
C
an
I
In
v)
mm
0
0
0
0
0
m
0
VIInw
ps
5:
0
zm
a
l­
4
d
s
eD
a3
51
3
h)
rl
7­
4
W
c
n
m
c
m
cu
.­
I
03
0
h
0
r(
r
r­
4
N
9
$
3
2
R
N
h)
3
l­
4
h)
N
B
0
0
0
00
0
00
0
0
0
0
0
m
L
3
U
u
m
W
Gl
m
hJ
W
W
.
c
c
W
C
c,
­
Y
5m
C
m
OI
e
cl
U
W
W
00
W
0
­
0
8
0
0
r
L
c
c
L
V
0
c
W
.
r
C
.­
u
N
W
L
C
c
eY­
II­:
W
O
I
c
*­
E
n
Y
0
0
D
W
WL
aoc
B
C
­
cc
1
rl
L
W
o­
r
u
om
u
I
80
000090
20
.­.
.
.

Method
Blonk
0
SpILed
Refettnce
firrue
0
Spiked
Reference
Tissue
­
Internet
OC
.
A
NHATS
FY
82
Composite
Spcimns
d­
chlaoform
I
1
I.
I
t
I
I
I
3I
9I
io
11
izI
13
16
17
ia
J
0
6/
19
21
zz
26
27
28
29
7/
2
I
I
I
I
I
I
Analysis
Dote
(
1984)

Atb2
a
0
r­
0
A
i
J000091
0
:
*
r
de­
toluene
A
A
A
b
A
8
A
A
A
a
A
b
A
b
A
A
1
I
1
1
I
I
I
.­
I
I
I
6/
19
21
22
2s
,27
29
29
712
3
9
Amlyrir
Dole
(
1981)

b
A
L
A
H
3
Ie
3 

3
Method
Blank
0
Spiked
Refereme
Tissue
0
Spiked
Reference
Tiwue
­
Internol
QC
A
NHATS
FY
82
Campolite
Specimens
A
A
A
AA
A
A
A8A
A
A
A
A
8
A
A
A
A
I
I
i
I
t
I
I
J
IO
II
12
13
16
17
ie
kth+
Blank
a
Splked
Reference
Tirrue
0
Splked
Rclercncs
litru.
­
Interno1
QC
A
NHATS
FY
82
Comporlte
Specimens
Figure
23.
Observed
HRGC/
MS
responses
for
the
internal
standards
dg­
toluene
and
dg­
chlorobenzene,
from
method
blanks,
spiked
tissue
samples
and
the
NHATS
composite
samples.

82
000092
20
kthod
8lonL
0
Spiked
Reference
Tissue
0
Spiked
Reference
Tirwe
­
lntcrnol
QC
A
NHATS
FY
82
Compoiite
Spcc;
meny
4r
01
1
I
I
1
I
I
I
I
I
I
1
I
I
I
1
1
f
J
6/
19
21
22
26
27
28
29
7/
2
3
9
10
II
12
13
16
17
18
20
Anolysii
Dote
(
1984)

Method
BIonk
0
SpIked
Reference
Tirsue
0
Spiked
Reference
Tiiswe
­
Internal
QC
A
NHATS
FY
82
Compoiite
Specimens
d
10­
ethyibenzene
A
A
01
I
f
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
6/
19
21
22
26
27
28
29
7/
2
3
9
IO
I1
12
13
16
17
IS
20
Amlyrii
Dote
(
1984)

Figure
24.
Observed
HRGC/
MS
responses
for
the
internal
standards
dig­
p­
xylene
and
dipethylbenzene,
from
method
blanks,
spiked
tissue
samples
and
the
,
NHATS
composite
samples.

83
000093
20
A
b
I
1
I
1
I
I
I
I
I
I
I
t
I
1
I
I
1
­
I­
IF
01
6/
19
21
22
26
27
28
29
7/
2
3
9
10
11
I2
13
16
17
18
J
Analysis
Doh
(
1964)

Mekhod
Blonk
0
Spiked
Reference
Tittw
0
Spiked
Reference
Tioue
­
lntcrnol
QC
a
"
ATS
FY
E2
Conlpogiie
Specinlcns
dq­
dichlorobenzene
­*­.­­*
­.­*­*­*
­*/*\.
I­
C..­*­­*
­.

m
2
0
I
I
I
1
I
I,
I
I
I
I
1
t
I
I
I
I
lj
6/'
l9
21
22
26
27
28
29
7/
2
3
9
IO
It
12
13
I6
li
18
10
Anolysis
Date
(
1964)

Figure
25.
Observed
HRGC/
MS
responses
for
the
internal
standards
d2­
l
,
l,
Z,
Z­
tetrachloroethane
and
dq­
dichl
orobenzene,
from
method
blanks,
spiked
tissue
samples
and
the
NHATS
composite
samples.
84
880094
VI.
REFERENCES
Balkon
3,
Leary
JA.
1979.
An
initial
report
on
a
comprehensive,
quantitative
screening
procedure
for
volatile
compounds
of
forensic
and
environmental
interest
in
human
biofluids
by
GC/
MS.
J
Anal
Toxicol
3:
213­
215.

Brown
RH,
Purnell
CJ,
1979.
Collection
and
Analysis
of
Trace
Organic
Vapor
Pollutants
in
Ambient
Atmospheres.
The
Performance
of
a
Tenax
Adsorbent
Tube.
178:
79­
90.

Corbett
TH.
1973.
Retention
of
anesthetic
agents
following
occupational
exposure
Anesth
Anal
52:
614.

Engstrom
K.
1984.
Styrene.
Chapter
10.
In:
Biological
monitoring
and
surveillance
of
workers
exposed,
to
chemicals.
Antero
A,
Riihimgki
V,
Vainio
H,
eds.
Hemisphere
Pub1ishing
Corp,
pp.
99­
110.

Engstrom
J,
Riihim'dki
V.
1979.
Distribution
of
m­
xylene
to
subcutaneous
adipose
tissue
in
short
term
experimental
human
exposure.
Scand
3
Work
Envi
ran
Health
5:
126­
134.

Hiatt
MH.
1983.
Determination
of
volatile
organic
compounds
in
fish
samples
by
vacuum
distillation
and
fused
silica
capillary
gas
chromatography/
mass
spectrometry.
Anal
Chem
55:
506­
516.

Karbowski
RJ,
Braun
WH.
1978.
Quantitative
determination
of
styrene
in
biological
samples
and
expired
air
by
gas
chromatography/
mass
spectrometry
(
selected
ion
monitoring).
J
Chromatog
160:
141­
145.

Lin
S­
N,
Fu
FW­
Y,
Bruckner
JV,
Feldrnan
S.
1982.
Quantitation
of
1,
l­
and
1,2­
dichloroethylene
in
body
tissues
by
purge­
and­
trap
gas
chromatography.
J
Chromatog
244:
311­
320.

Lucas
RM,
Pierson
SA,
Myers
DL,
Handy
RW.
1981.
National
Human
Adipose
Tissue
Survey
Quality
Assurance
Program
Plan,
Preliminary
Draft,
RT1/
1864/
21­
11.

Luskus
LJ,
Kilian
HJ,
Lackey
WW,
Biggs
JD.
1977:
Gases
released
from
tissue
'

and
analyzed
by
infrared
and
gas
chromatography/
mass
spectroscopy
techniques.
3
Forsenic
Sci
22(
3):
500.

Mack
GA,
Stanley
J.
1984.
Preliminary
strategy
on
the
National
Human
Adipose
Tissue
Survey.
Washington,
DC:
Office
of
Toxic
Substances,
Contracts
68­
016721
(
Task
21)
and
68­
02­
3938(
Work
Assignment
8).

Michael
LC,
Erickson
MD,
Parks
SP,
Pellitzari
ED.
1980.
Volatile
environmenta
pollutants
in
biological
matrices
with
a
headspace
purge
technique.
Anal
Chem
52:
1836­
1841.

Novotny
My
McConnell
ML,
Lee
Mt,
Farlow
R.
1974.
High­
resolution
gas­
chromatographic
analysis
of
the
volatile
constituents
of
body
fluids,
with
use
of
glass
capillary
columns.
Clin
Chem
20(
9):
1105­
1110.
.
Pantarotto
Cy
Fanelli
R,
Belletti
I,
Bidoli
F.
1980.
Determination
of
styrene
in
biological­
specimens
by
gas
chromatography­
selected
ion
monitoring:
distribution
in
mice.
Anal
Biochem
105:
340­
347.

Peoples
AJ,
Pfaffenberger
CD,
Enos
HF,
Shafik
TM.
1978.
An
LSC/
GLC/
ECD
method
for
quantifying
human
serum
and
adipose
tissue
levels
of
volatile
purgeable
halogenated
hydrocarbons.
Am
Chem
SOC
Div
Environ
Chem
18(
2):
485­
486.

Peoples
AJ,
Pfaffenberger
CD,
Shafik
TM,
Enos
HF.
1979.
Determination
of
volatile
purgeable
halogenated
hydrocarbons
in
human
adipose
tissue
and
blood
serum.
Bull
Environm
Contam
Toxicol
23:
244­
249.

Pfaffenberger
CD,
Freal
53,
111.
1979.
A
convenient
purging
device
for
analyzing
adipose
tissue
for
volatile
components.
J
HRC
&
CC
10114.

Politzer
IR,
Githens
S,
Dowty
BJ,
Laseter
JL.
'
1975.
Gas
chromatographic
evaluation
of
the
volatile
constituents
of
lung,
brain
and
1i"
ver
tissues.
J
Chromatog
Sci
13:
378­
379.

Reddrop
CJ,
Riess
W,
Slater
TF.
1980.
Two
rapid
methods
for
the
simultaneous
gas­
liquid
chromatographic
determination
of
carbon
tetrachloride
and
chqaroform
in
biological
material
and
expired
air.
J
Chromatog
193:
71­
82.

Reinert
KH,
Hunter
JV,
Sabatino
T.
1983.
Dynamic
heated
headspace
analyses
of
volatile
organic
compounds
present
in
fish
tissue
samples.
J
Agric
Food
Chem
31:
10'
57­
1060.

Stanley
JS.
1986a.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
I;
Executive
Summary.
EPA­
560/
5­
86­
035.

Stanley
JS.
1986b.
Broad
scan
analysis
of
human
adipose
t
ssue:
Volume
11:
Volatile
organic
compounds.
EPA
560/
5­
86­
036.

Stanley
35.
'
1986~.
Broad
scan
analysis
of
human
adipose
t
ssue:
Volume
111:
Semivolatile
organic
compounds.
EPA
560/
5­
86­
037.

Stanley
JS.
1986d.
Broad
scan
analysis
of
human
adipose
t
ssue:
Volume
N:
Polychlorinated
dibenzo­
pdioxins
(
PCDDs)
and
polychlorinated
dibenrofurans
(
PCDFs).
EPA­
560/
5­
86­
038.

Snyder
CAY
Erlichman
MN,
Goldstein
BD,
Laskin
S.
1977.
An
extraction
method
for,
determinationof
benzene
in
tissue
by
gas
chromatography.
Am
Ind
Hyg
ASSOC
J
38:
272­
276.

USEPA.
1984.
U.
S.
Environmental
Protection
Agency.
Method
624­­
purgeables.
(
49
FR
141­
152).

Vogt
CR,
Liao
JC,
Sun
AY.
1980.
Extraction
and
determination
of
chloroform
in
rat
blood
and
tissues
by
gas
chromatography­
electron­
capture
detection:,
distribution
of
chloroform
in
the
animal
body.
Clfn
Chem
26(
1):
66­
68.

86'

000096
Whitcher
CE,
Cohen
EN,
Trudell
JR.
1971.
Chronic
exposure
to
anesthetic
gases
in
the
operating
room.
Anesth
35:
349.

Wolff
MS.
1976.
Evidence
of
existence
in
human
tissues
of
monomers
for
plastic
and
rubber
manufacture.
Environ
Health
Perspect
17:
183­
187.

Wolff
MS,
Daum
SM,
Loumer
WV,
Selikoff
13,
Aubrey
BB.
1977.
Styrene
and
related
hydrocarbons
in
subcutaneous
fat
from
polymerization
workers.
Toxicol
Environ
Health
2:
997­
1005.

Zuccato
E,
Marcucci
F,
Mussini
E.
1980.
GLC
determination
of
ethylene
dichloride
(
EDC)
in
biological
samples.
Anal
Ltr
13(
B5):
363­
370.

87
00009'
7
APPENDIX
A
ANALYTICAL
METHOD
FOR
THE
DETERMINATION
OF
VOLATILE
ORGANIC
COMPOUNDS
IN
HUMAN
ADIPOSE
TISSUE
A­
I
ANALYTICAL
METHOD
FOR
THE
DETERMINATION
OF
VOLATILE
ORGANIC
COMPOUNDS
IN
HUMAN
ADIPOSE
TISSUE
1.0
SCOPE
AND
APPLICATION
1.1
This
method
covers
the
determination
of
volatile
organic
compounds
in
human
adipose
tissue:
The
following
compounds
have
been
evaluated
and
determined
by
this
method.

Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To
1
uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1,4­
Dichlorobentene
Ethyl
phenol
Xylene
CAS
no.

67­
66­
3
71­
55­
6
75­
27­
4
71­
43­
2
127­
18­
4
124­
48­
1
79­
00­
5
108­
88­
3
108­
90­
7
100­
41­
4
75­
25­
2
100­
42­
5
79­
34­
5
95­
50­
1
106­
46­
7
25429­
37­
2
1330­
20­
7
~

1.2
This
is
a
dynamic
headspace
high
resolution
gas
chromatography/
.
mass
spectrometry
(
HRGC/
MS)
method
applicable
to
the
determination
of
volatile
organic
compounds
in
human
adipose
tissue.'

1.3
The
method
detection
limit
(
MDL)
for
each
parameter
is
estimated
to
range
from
0.001­
0.10pg/
g
for
a
20­
9
sample.
The
MDL
for
a
specific
sample
of
human
adipose
tissue
may
differ
depending
upon
the
nature
of
interferences
in
the
sample
matrix
and
the
specific
analyte
determined.

2.0
METHOD
SUMMARY
Helium
gas
is
swept
through
the
head
space
of
a
special.
1ydesigned
purging
chamber
containing
water
and
the
adipose
tissue
sample.
The
water
and
sample
are
heated
and
stirred
to
aid
in
the
efficient
transfer
of
the
analytes
from
the
adipose
tissue
and
water
mixture
to
the
gaseous
phase.
The
vapor
is
swept
through
a
cooling
tower,
atambient
temperature
to
remove
excess
water
vapor
and
onto
a
Tenax
sorbent
trap
where
the
volatile
analytes
are
captured.
After
the
sampling
is
complete
the
sorbent
trap
is
heated
and
backflushed
with
helium
to
desorb
A­
2
000099
the
analytes
onto
a
HRGC
column.
The
gas
chromatograph
is
temperature
programmed
to
separate
the
compounds
which
are
then
detected
by
the
mass
spectrometer.
Figure
A­
1
provides
a
schematic
of
the
dynamic
head­
space
purge
and
trap
HRGC/
MS
analysis
system.

3.0
CONTAMINATION
AND
INTERFERENCES
3.1
'
Impurities
in
the
purge
gas,
organic
compounds
out­
gassing
from
the
plumbing
upstream
of
the
trap,
and
solvent
vapors
in
the
laboratory
account
for
the
majority
of
contamination
problems.
The
analytical
system
is
demonstrated
to
be
free
from
interferences
under
conditions
of
the
analysis
by
analyzing
blanks
initially
and
with
each
sample
set
analyzed
daily.

3.2
Samples
can
be
contaminated
by
diffusion
of
volatile
organic
compounds
through
the
bottle
seal
during
preparation,
handling,
or
storage.
A
sample
container
blank
carried
through
the
sampling
and
handling
protocol
serves
as
a
check
on
such
contamination.

3.3
Contamination
by
carry­
over
can
occur
when
high
level
and
low
level
samples
are
analyzed
sequentially.
To
reduce
carry­
over,
a
clean
headspace
chamber
is
used
for
each
sample
analysis
and
sample
syringes
are
rinsed
between
samples
with
reagent
water.
Instrument
performance
checks
and
QC
samples
are
followed
by
analysis
of
a
reagent
water
blank
to
check
for
carry­
over'.
The
headspace
device
is
washed
with
soap
solution,.
rinsed
with
tap
and
distilled
water,
and
dried
in
an
oven
at
10O­
12S0C
overnight.
The
Tenax
adsorbent
trap
and
other
parts
of
the
system
are
also
subject
to
contamination;
therefore,
frequent
bakeout
and
purging
of
the
entire
system
may
be
required.

3.4
Interferences
resulting
from
samples
may
vary
considerably,
depending
on
the
length
of
sample
storage.

4.0
SAFETY
4.1
The
toxicity
or
carcinogenicity
of
each
compound
used
in
this
method
has
not
been
precisely
def
ined;
however
,
each
compound
should
be
treated
as
a
potential
health
hazard.
Exposure
to
these
chemicals
should
be
maintained
at
the
lowest
possible
level.

4.2
The
glass
purging
apparatus
used
in
this
method
is
of
fairly
recent
design
and
has
apparent
limitations
which
must
be
observed.
The
pressure
in
the
system
should
not
exceed
10
psi.
Excessive
pressure
above
this
limit
may
result
in
the
possible
explosion
of
the
purging
vessel
or
purge
tower.
Monitoring
the
gas
pressure
is
easily
accomplished
by
placing
a
pressure
gauge
between
the
helium
source
and
the
gas
inlet
at
the
vessel.
At
no
time
should
any
glassware
be
pressurized
without
the
analyst
wearing
approved
safety
goggles.

A­
3
A­
4
5.0
APPARATUS
AND
MATERIALS
5.1
Gas
pressure
gauge
­
Supelco
No.
2­
0392
or
equivalent.

5.2
Spatulas,
stainless
steel
­
Fisher
No.
14­
375­
10.

5.3
Volumetric
flask
5.4
Syringes,

5.4.1
Syringe
5.4.2
Syringe
5.4.3
Syringe
5.4.4
Syringe
5.4.5
Syringe
5.5
Vials
­
2
x
5.0
mt
10.0
mL
­
Ace
No.
7100­
02.

10.0
mL
­
Hamilton
No.
1010.

1.0
mL
­
Hamilton
No.
1001.

100.0
pL
­
Hamilton
No.
710N.

25.0
yL
­
Hamilton
No.
702N.

2
x
5.0
pL
­
Hamilton
No.
75N.

microreaction
vessels
­
Supelco
No.
3­
3298.

5.6
Vials
­
2
x
1.0
mL
microreaction
vessels
­
Supelco
No.
3­
3292.

5.7
Mininert
valves
­(
x2)
­
Supelco
No.
3­
3301.

5.8
leflon@
tubing
(
1/
8­
in.
ID)
­
Ace
No.
12687­
08.

5.9
Funnel
(
1.0
L)
­
Ace
No.
.7249­
40.

5.10
Three­
way
stopcock
­
Ace
No.
8143­
05.

5.11
Vinyl
tubing
­
Ace
No.
12679­
24.

5.12
Hot
water
bath/
circulator
­
HAAKE
No.
F­
4391.

5.13
Teflon@
stir
bars
­
Ace
No.
13654­
10.

5.14
Stirrer
­
Ace
No.
13635.

5.15
Heat
tape
­
Ace
No.
12064­
08.

5.16
Powerstat
­
Ace
No.
12077.

5.17
Headspace
vessel
­
Wheaton
No.
991765.

5.18
Kovar
to
PX
seal
tubes
­
Ace
No.
Pt.
976.

5.19
Stainless
steel
tubing
­
Supelco
No.
2­
0526.
.

5.20
.
Six­
way.
Carle
valve.

A­
5
000102
5.21
Stainless
steel
glass
lined
U­
tube
(
1/
8
in.
ID).

5.22
Chromatography
gravity
flow
column
­
Howe
Scient.
Inc.,
No.
3060­
13
"
purge
tower".

5.23
Heat
controller
and
thermocouple.
I
5.24
Glass
wool
"
silanized".

5.25
HRGC
column
(
30
m
x
0.25
mm
ID)
Durabond
DB­
5,
0.25
pm
film
thickness
(
J&
W
Scientific,
Rancho
Cordova,
CA)
or
equivalent.

5.26
Gas
chromatograph
­
Finnigan
9610
or
equivalent
capable
of
maintaining
3OoC
isothermal
and
programmable
to
200OC.
The
gas
chromatograph
must
be
equipped
with
a
Grob
split/
splitless
type
injector.

5.27
Mass
spectrometer
­
Finnigan
4000
quadrupole
or
equivalent,
70
eV
electron
impact
ionization;
capable
of
repetitive
scan
from
35­
275
amu
every
2­
3
s,
and
produce
a
unit
resolution
(
valleys
between
m/
z
174­
176
less
than
10
percent
of
the
height
of
the
m/
z
175
peak),
background
corrected
mass
spectrum
from
50
ng
4­
bromo­
fluorobenzene
(
BFB)
injected
into
the
GC.
The
BFB
spectrum
must
meet
the
mass
intensity
criteria
in
Table
A­
1.
All
portions
of
the
HRGC
column,
transfer
lines,
and
the
HRGC
column
routed
directly
to.
the
ion
source
shall
remain
at
or
above
­
the
column
temperature
during
analysis
to
preclude
condensation
of
less
volatile
compounds.

Table
A­
1.
BFB
Mass
Intensity
Specifications
Mass
50
75
95
96
173
174
176
177
__­

Intensity
required
15
to
40
percent
of
mass
95.
30
to
60
percent
of
mass
95.
base
peak,
100
percent.
5
to
9
percent
of
mass
95.
<
2
percent
of
mass
174.
>
50
percent
of
mass
95.
95
to
100
percent
of
mass
174.
5
to
9
percent
of
mass
176.

5,28
Data
system
­
Capable
of
collecting
and
recording
MS
data,
storing
mass
intensity
data
in
spectral
libraries,
processing
HRGC/
MS
data
and
generating
quantitation
reports,
and
calculating
and
recording
response
factors.

\

A­
6
000103
4
'
i
I
..:
..
,.
.
_..
.
,
I'
.
,.~
.
,.

5.28.1
Data
acquisition
­
Mass
spectra
shall
be
collected
continuously
throughout
the
analysis
and
stored
on
a
mass
storage
device.

5.28.2
Mass
spectral
'
libraries
­
User
created
libraries
containing
mass
spectra
obtained
from
analysis
of
authentic
standards
must
be
used
to
reverse
search
GUMS
runs
for
the
compounds
of
interest.

5.28.3
Data
processing
­
The
data
system
shall
be
used
to
search,
locate,
identify,
and
quantitate
the
compounds
of
interest
in
each
HRGC/
MS
analysis.
Software
routines
shall
be
employed
to
compute
retention
times
and
extracted
ion
current
plot
(
EICP)
areas.
Displays
of
spectra,
mass
chromatograms,
and
library
comparisons
are
required
to.
verify
results.

5.28.4
.
Response
factors
and
multi­
point
calibrations
­
The
data
system
shall
be
used
to
record
and.
maintain
lists
of
response
factors
(
response
ratios
for
isotope
dilution)
and
generate
multi­
point
calibration
curves.
Computations
of
relative
standard
deviation
(
coefficient
of
variation)
are
useful
for
testing
calibration
linearity.

5.29
Balance
­
Ana'lytical,
capable
of
weighing
0.1mg.

6.0
REAGENTS
6.1
Volatile
organic­
free
water
­
prepare
as
described
in
Section
8.1,

6.2
Prepurified
nitrogen.

6.3
Prepurified
he1i
urn.

6.4
Tenax
absorbent.

6.5
Internal
standard
compounds
6.5.1
Bromochloromethane,
1,4­
dichlorobutane,
and
I­
chloro­
2bromopropane
(
a
ZO­
mg/
mL
mixture,
Supelco,
Inc.,
No.
4­
0823).

6.5.2
.
d6­
Benzene
­
Aldrich
gold
label
(
99.5%
0)
No.
15,
181­
5.

6.5.3
d­
Chloroform
­
Aldrich
gold
label
(
99.8%
0)
No.
15,
182­
3.

6.5.4
d2­
1,1,2,2­
Tetrachloroethane
­
M
and
D
Isotopes
No.
MD­
1416.

6.5.5
d,­
Methylene
chloride
­
M
and
D
Isotopes
No.
MD­
53.

A­
7
000104
6.5.6
d,­
Chlorobenzene
­
KOR
Isotopes
(
99%
D,)
No.
521510.

6.5.7
1,4­
d4­
Dichlorobenzene­
KOR
Isotopes
(
98%
0,)
No.
521530.

6.5.8
dlo­
Ethylbenzene­
KOR
Isotopes
(
98%
Dlo)
No.
521443.

6.5.9
d8­
Toluene
­
KOR
Isotopes
(
99.9%
D,)
No.
510041.

6.5.10
dlo­
p­
Xylene­
KOR
Isotopes
(
98%
Dlo)
No.
521133.

6.6
Target
analytes
6.6.1
Bromoform
­
Aldrich
gold
label
(
99%/
l%
EtOH)
(
d
2.894
g/
mL).

6.6.2
Dibromochloromethane
­
Columbia
No.
D1843
(
d
2.45
g/
mL).

6.6.3
Toluene
­
Burdick
and
Jackson
H.
P.
No.
A1­
857
(
d
0.867
g/
mL).

6.6.4
1,1,2­
Trichloroethane­
Aldrich
No.
J6­
070177
(
95%)
(
d
1.435
g/
mL).

6.6.5
Styrene
­
Eastman
No.
1465
(
d
1.34g/
mL).
I
6.6.6
Tetrachloroethene
­
Aldrich
gold
label
No.
120457
(
d
1.54
g/
mL).

6.6.7
Bromodichloromethane
­
Aldrich
No.
7628AH
(
98%)
(
d
1.49
g/
rnL
1.

6.6.8
Chlorobenzene
­
Aldrich
No.
120277
(
99%)
(
d
1.107
g/
mL).

6.6.9
1,2­
Dichlorobenzene­
Aldrich
No.
D5­
680­
2(
98%)
(
d
1.306
g/
mL).

6.6.10
Ethylbenzene
­
Aldrich
No.
E1­
250­
8(
99%)
(
d
0.867g/
mL).

6.6.11
1,1,2,2­
TetraChloroethane
­
Baker
No.
017386
(
d
1.586
g/
mL).

6.6.12
l,
l,
l­
Trichloroethane­
Fisher
No.
775974
(
d
1.338g/
mL).

6.6.13
Chloroform
­
Burdick
and
Jackson
H.
P.
No.
AG594
(
d
1.492
g/
mL).

6.6.14
Benzene
­
MCB
pest.
grade
No.
U2738
(
d
0.874g/
mL).

6.7
Methanol
­
Burdick
and
Jackson,
high
purity
distilled
in
glass.

6.8
Tetraglyme
­
Aldrich
17­
240­
5.

6.9
Acetone
­
Burdick
and
Jackson,
high
purity
distilled
in
glass.

6.10.
Hexane
­
Burdick
and
Jackson,
high
purity
distilled
in
glass.

A­
a
000105
I_
7.0
8.0
HEADSPACE
APPARATUS
PREPARATION
7.1
.
Glassware
preparation
­
All
glassware
is
washed
with
a
laboratory
grade
soap
(
i.
e.,
Sparkleen
or
equivalent)
and
rinsed
with
deionized
water,
bulk
grade
acetone,
B&
J.
acetone,
and
finally
B&
J
hexane.
The
glassware
is
air
dried
to
remove
traces
of
hexane
and
then
dried
in
an
oven
at
2OO0C
for
48
h
before
use.

7.2
Wheaton
purge
vessel
­
The
Wheaton
purge
vessel
thermometer
and
funnel
arms
were
modified
as
follows.
The
threaded
arms
were
cut
near
the
vessel
and
replaced
by
1/
4­
in.
Kovar@
to
PX
seal
tubes
(
Ace
Glass,
Inc.,
No.
PT.
976).
The
KovarB
length
was
1.0
in.
The
arms
were
made
as
short
as
possible
to
minimize
dead
volume.
The
vessel
is
integrated
in
the
system
as
in
Figure
A­
1.

7.3
Chromatographic
gravity
flow
column
(
purge
tower)
­
The
column
is
connected
to
the
system
as
displayed
in
Figure
A­
1.
Two
milliliters
of
volatile
organic­
free
water
is
placed
in
the
tower
to
trap
excess
water
vapor.

7.4
Glass­
lined
U­
tube
sorbent
trap
­
A
1.0­
in.
plug
of
Tenax
is
placed
in
the
tube,
and
a
plug
of
silanized
glass
wool
placed
at
both
ends.
Do
not
overpack
the
Tenax.
Pack
only
tight
enough
to
avoid
any
dead
volume
in
the
Tenax.
Overpacking
will
make
it
difficult
to
maintain
a
40.0­
mL/
min
helium
flow
under
the
10.0
psi
safety
pressure.

Refer
to'Figure
A­
1
for
a
detailed
orientation
of
all
system
components

REAGENT
PREPARATION
8.1
Volatile­
free
water
­
Volatile
organic
compounds
are
purged
from
water,
taken
from
the
Millipore
system;
by
bubbling
the
prepurified
nitrogen
through
the
water
for
24
h
prior
to
use.

8.2
Internal
standard
preparation
.

8.2.1
Internal
standard
stock
solution
­
The
internal
standard
stock
solution
is
prepared
from
compounds
6.5.2
through
6.5.10
by
a1iquotting
each
compound
with
a
100.0­
pL
syringe
into
a
10.0­
mL
volumetric
containing
5.0
mL
of
methanol.
The
exact
volume
of
each
target
analyte
necessary
to
achieve
a
final­
concentration
of
10
mg/
mL
for
each
compound
can
be
determined
from
the
density
of
the
compound.
After
aliquotting
all
compounds,
dilute
to
the
mark
with
the
methanol.
Transfer
the
10.0­
mt
solution
to
two
5.0­
mL
vials
and
seal
tightly
with
the
TFE­
lined
caps.
Store
in
the
freezer
until
needed.

A­
9
8.2.2
Internal
standard
spi
king
solution
­
A
500­
ng/
yL
internal
standard
spiking
solution
is
prepared
in
tetraglyme
by
injecting
925.0
pL
of
tetraglyme
into
a
1.0­
mL
reaction
vial
with
mininert
cap.
This
is
then
spiked
with
25.0­
pL
of
the
3­
component
(
20
mg/
mL)
Supelco
standard
and
50.0­
pL
of
the
lO.
O­
mg/
mL
internal
standard
stock
of
8.2.1.
Store
in
the
freezer
until
needed.

8.3
Target
analyte
preparation
8.3.1
Target
analyte
stock
solution
­
A
lO.
O­
mg/
mL
each
solution
of
the
analytes
from
6.6.1
through
6.6.14
is
prepared
as
described
for
the
internal
standard
stock
solution
in
8.2.1.
Store
in
the
freezer.

8.3.2
Target
analyte
spiking
solution
­
A
100.0­
ng/
pL
solution
of
each
of
the
target
analytes
is
prepared
by
injecting
990.0
VL
of
tetraglyme
into
a
1.
O­
mL
reaction
vial
with
mininert
cap
and
spiking
the
tetraglyme
with
10.0
pL
of
the
stock
solution
of
8.3.1.
Store
in
the
refrigerator.

ANALYSIS
ROUTINE
This
routine
must
be
followed
after
any
system
shutdown
or
at
least
once
every
8
h
prior
to
any
sample
analysis.

9.1
Perform
an
instrument
mass
calibration
using
bromofluorobenzene
(
BFB)
to
achieve'the
mass
intensity
specifications
in
Table
A­
1.

9.2
Conduct
a
purge
tower
instrument
evaluation
with
the
system
set
up
as
in
Figure
A­
1.

9.2.1
Conduct
a
leak
test
by
squirting
VOA­
free
water
around
,
all
connections,
vessel
cap,
etc.
Correct
as
needed.
Check
the
bubble
meter
for
the
correct
40.0­
rnL/
min
flow.
The
Carle
valve
must
be
in
the
purge
position.

9.2.2
Turn
off
the
purge
tower
stopcock
and
immediately
turn
the
helium
supply
off.
Check
the
pressure
gauge
for
a
slow
pressure
falloff.
If
the
gauge
reading
drops,
check
again
for
leaks.

9.2.3
Remove
the
purge
tower
cap.

9.2.4
Connect
a
30­
cm
length
of
Teflon@
tubing
to
the
10.0­
mL
syringe.
Draw
3.0
mL
of
VOA­
free
water
into
the
syringe.
Remove
the
Teflon@
tubing
and
draw
1.0
mL
of
air
into
the
syringe.
Using
two
separate
5.0­
pL
syringes,
withdraw
2.0
pL
of
each
working
solution
of
8.2.2
and
8.3.2.
Spike
the
10.0
mL
syringe
with
each
of
the
standard
spiking
A­
10
.
000107
9.0
solutions.
Be
sure
to
inject
directly
into
the
water.
Reseal
the
mininert
valves
and
return
the
standards
to
a
refrigerator.
Replace
the
Teflon@
tubing
on
the
10.0­
mL
syringe.
Invert
the
syringe
several
times
to
ensure
adequate
mixing
of
the
tetraglyme
and
water.

9.2.5
Inject
the
contents
of
the
10.0­
mL
syringe
directly
into
the
water
at
the
bottom
of
the
purge
tower.
The
air
in
the
syringe
should
push
the
water
solution
completely
out,
but
should
not
be
allowed
to
bubble
out
the
end
of
the
Teflon@
tube.
Immediately
withdraw
the
Teflon@
tube
and
recap
the
purge
tower.

9.2.6,
With
the
Carle
valve
in
the
purge
mode,
the
Tenax
trap
at
ambient
temperature,
and
all
heat'
tape
lines
at
15OoC,
turn
on
the
helium
supply
valve
and
then
the
stopcock
at
the
purge
tower.

NOTE:
If
the
stopcock
on
the
purge
tower
is
left
closed,
the
helium
gas
.
may
rupture
the
purge
vessel.

Check
the
system
for
leaks.
Ifa
leak
is
detected,
the
system
must
be
shut
down
and
the
purge
tower
cleaned
as
out1ined
below.

9.2.7
Purge
the
purge
tower,
for
12
min
at
40
mL/
min.

9.2.8
After
the
purge
is
complete,
turn
the
Carle
valve
to.
the
desorb
mode,
heat
the
Tenax
trap
to
approximately
25OoC
and
initiate
the
HRGC/
MS
data
acquisition.
These
three
procedures
are
done
as
quickly
as
possible
to
maintain
the
absolute
retention
times
between
analysis.
The
gas
~

chromatograph
should
be
held
isothevmal
at
3OoC
for
5
min
then
programmed
to
125OC
at
6OC/
min.
Hold
at
125
°
C
for
10
min
and
then
program
to
2OO0C
before
returning
to
3OOC.

4
9.2.9
During
the
HRGC/
MS
data
acquisition,
remove
the
purge
tower
cap
and
rinse
the
tower.
Using
the
10.0­
mL
syringe
and
Teflon@
tube,
alternately
add
and
withdraw
10,
O­
mL
portions
of
VOA­
free
water.
Repeat
this
procedure
a
minimum
of
six
times
and
discard
each
rinse.
Reassemble
the
tower
with
2.0
mL
of
VOA­
free
water.

9.2.10
After
data
acquisition
is
complete,
check
the
HRGC/
MS
response
to
the
internal
standards.
Note
that
often
the
initial
analysis
of
the
system
following
instrument
shutdown
will
give
variable
responses.
If
this
is
observed
and
the
responses
are
not
equivalent
to
that
previously
regarded
as
optimum
performance,
the
purge
tower
instrument
evaluation
must
be
repeated.
Refer
to
Calculations
(
Section
11.0)
for
response
factor
calculations.
Figure
A­
2
is
an
example
of
an
HRGC/
MS
chromatogram
obtained
for
an
instrument
performance
check.

A­
11
0003.08
1.
Benzene/
dg­
benrene
2.
Bromodichforomethane
8.
9.
d
10­
e
thy1benzene
Ethylbentene
3.
To
Iuene/
d8­
to
Ive
ne
10.
dio­
p­
xyle
ne
4.
Bromochloropropane/
11.
Brornoform
1,
i,
2­
trichloroethane
12.
Styrene
5.
Dibrornochloromethane
13.
Dic
hlorobutane
6.
Tetrachloroethe
ne
7.
Ch
lorobentene/
14.
15.
1,1,2,2­
tetrochloroethane
d4­
1,4­
dichlorobenzene
dg­
chlorobenzene
16.
1,2­
dichlorobenzene
Purge
Tower.
5
tandurd
1W.
l
1
1
.'
,

4
4
f
16
12
1
6
Figure
A­
2.
HRGC/
MS
chroma
togram
of
purge
tower
standard
analyzed
daily
to
document
instruhent
performance.

A­
12
000109
9.3
External
quality
control
check
­
External
quality
control
checks
(
blind
samples)
should
be
conducted
by
the
project
Quality
Control
Coordinator
(
QCC)
to
demonstrate
proper
instrument
calibration.
These
QC
checks
are
performed
periodically
(
typically
on
the
first
analysis
day
of
each
week).

9.3.1
Allow
the
Tenax
trap
to
return
to
room
temperature.

9.3.2
The
Q'C
check
is
conducted
in
the
same
manner
as
the
purge
tower
instrument
check,
but
the
target
analyte
spiking
solution
is
provided
by
the
project
Quality
Control
Coordi
nator
(
QCC
1.

9.3.3
The
recoveries
of
the
target
ana?
ytes
are
calculated
and
provided
to
the
QCC
for
evaluation.
If
the
evaluation
is
adequate,
the
analyst
proceeds
with
the
system
blank
after
completing
the
system
rinse
as
in
9.2.9.
If
the
QC
check
does
not
demonstrate
acceptable
performance,
the
analyst
must
recalibrate
the
system
and
repeat
the
QC
check.

9.4
System
blank
9.4.1
With
the
system
set­
up
as
in
Figure
A­
1,
with
the
Carle
valve
in
purge
mode,
add
80.0
mL
of
VOA­
free
water
in
the
Wheaton
vessel
and
check
for
leaks.

9.4.2
Turn
the
purge
tower
valve
off
and
helium
supply
off.

9.4.3
Remove
the
Wheaton
vessel
cap
and
inject
2.0
pL
of
the
internal
standard
solution.
Follow
9.2.4,
but
substitute
the
vessel
for
the
purge
tower
and
omit
the
analyte
solution

9.4.4
Reseal
the
vessel,
turn
on
the
helium
at
the
helium
supply
valve.
When
a
pressure
reading
is
observed
in
the
system,
open
the
stopcock
at
the
purge
tower;
this
will
prevent
water
from
seeping
into
the
lines
at
the
bottom
of
the
purge
tower.
Check
for
leaks.

9.4.5
Turn
on
the
stirrer
and
the
valve
at
the
three­
way
hot
water
junction,
so
that
the
heated
(
95OC)
water
will
flow
through
the
vessel
jacket.
Purge
the
system
for
40.0
min.

9.4.6
After
the
40.0­
min
purge,
desorb
as
in
9.2.8.

9.4.7
Remove
the
modified
Wheaton
vessel
and
replace
with
a
clean
headspace
apparatus
containing
80.0
mL
VOA­
free
water
and
clean
stirring
bar.

A­
13
9.4.8
Determine
the
level
of
contaminants
and
record.
If
excessive
background
is
observed,
clean
the
purge
tower,
the
transfer
lines
and
repeat
the
system
blank
using
a
clean
headspace
apparatus.

9.5
Tissue
standard
­
A
tissue
sample
(
20
g)
spiked
with
known
levels
of
the
series
of
target
analytes
and
internal
standards
should
be
analyzed
daily
to
document
relative
response
factors
from
the
tissue
matrix.
Prior
to
initiating
actual
sample
analysis,
the
analyst
should
analyze
a
series
of
adipose
tissue
samples
spiked
with
0.20
to
1.4
pg
of
each
of
the
target
analytes
and
1.0
pg
of
each
internal
standard.
The
analyst
should
require
a
relative
response
factor
consistency
of
It
40%
variability
for
the
Calibration
curve
and
for
day
to
day
verification
of
the
calibration.
If
the
measured
response
factors
are
determined
to
vary
by
more
than
40%
of
the
average,
the
calibration
curve
must
be
re­
established
The
analyst
must
be
aware
that
the
background
contribution
of
the
tissue
selected
for
spiked
samples
will
effect
the
measured
response
factors.
If
the
background
contribution
is
significant,
the
analyst
must
analyze
an
unspiked
sample
to
determine
the
level
of
background.
Figure
A­
3
is
an
example
of
a
spiked
tissue
standard.

9.5.1
With
the
system
as
in
Figure
A­
1,
turn
off
the
purge
tower
stopcock
and
helium
supply
valve.
Remove
the
Wheaton
vessel
cap
and
place
20.0
g
of
frozen
adipose
tissue
in
the
80.0
mL
of
water.
Use
the
Fisher
spatula
to
manipulate
the
frozen
tissue.
The
adipose
tissue
used
for
the
tissue
standard
analysis
should
be
from
a
bulk
supply
so
that
each
tissue
standard
will
be
subjected
to
the
same
matrix
effects.
Recap
the
vessel.

9.5.2
Spike
this
solution
with
2.0
pL
of
each
spike
solution
as
in
9.2.4.
Quickly
recap
the
vessel.

9.5.3
Turn
on
the
helium
supply
valve
and
open
the
purge
tower
stopcock.
Be
sure
the
Carle
valve
is
in
the
purge
position
and
the
Tenax
trap
is
at
ambient
temperature.
Check
for
leaks.

9.5.4
Purge
the
vessel
for
40
min.
After
the
40
min,
desorb
as
in
9.2.8.

9.5.5
During
data
acquisition,
clean
and
replace
the
Wheaton
vessel.

9.5.6
Check
the
instrument
'
response
to
the
internal
standard
compounds.
Calculate
the
response
factor
for
each
target
analyte
versus
the
respective
internal
standard
and
record.

A­
14
.
.
..
.
'.
:..'
,
,..
.
.....
,
..
.',
;.
,
.
...

1
.
Ch1oroform/
d­
c
hI
oroform
2.
Bromachloromethans
3.
1,1,
I­
trichloroethane
4.
Benzene/
dg­
benzene
5.
Bromodi
c
hIorom&
hane
6.
ToI
ueneidg­
to
I
we
ne
7.
1,1,2­
trichloroethane
8.
DibromochIoromethane
9,
Tetrachloroethene
10.
Chlorobenzene/
dg­
ch
lorobenzene
11.
dlpethylbenzene
12.
Ethylbenzene
13.
dlpp­
xylene
14.
Bromoform
15.
Styrene
16.
1,1,2,2­
tetrachioroethane/
d2­
l11,2,2­
tetrachloroethane
17.
d4­
1
,
I­
dichlorobenzene
18.
I
,2­
dichlorobenzene
Tissue
Stondard
9
BIC.

P
8
C­
F
i
19lee
Figure
A­
3.
HRGC/
MS
chromatogram
for
the
volatile
organic
analysis
of
a
bulk
'
adipose
tissue
spiked
'
with
1
.
O
UCJ
of
each
internal
standard
and
0.20
uq
of
each
target
analyte.

A­
15
080112
­.
9.6
Sample
analysis
9.6.1
Sample
analysis
is
achieved
exactly
the
same
manner
as
the
tissue
standard
with
the
exception
that
the
target
analyte
spiking
solution
is
omitted.
Figure
A­
4
is
an
example
of
the
volatile
organic
analysis
of
a
composite
adipose
tissue
sample
analyzed
with
the
National
Human
Adipose
Tissue
Survey
Fiscal
Year
1982
samples.

9.6.2
Checking
the
instrument
response
after
each
acquisition
and
before
proceeding
to
the
next
analysis
will
help
prevent
the
loss
of
valuable
samples.

10.0
QUALITATIVE
IDENTIFICATION
Obtain
EICPs
for
the
primary
quantitation
ion
and
at
least
one
secondary
masses
for
each
parameter
of
interest.
The
following
criteria
must
be
met
to
make
a
qualitative
identification.
Table
A­
2
provides
a
summary
of
the
primary
quantitation
ions
and
the
HRGC
characteristics
for
each
of
the
target
analytes
and
internal
standards.

10.1
The
characteristic
masses
of
each
parameter
of
interest
must
maximize
in,
the
same
or
within
one
scan
of
each
other.

10.2
The
retention
time
must
fa.
11
within
?
I
30
s
of
the
retention
time
of
the
authentic
compound.

10.3
The
relative
peak
heights
of
the
characteristic
masses
in
the
EICPs
must
fall
within
&
20%
of
the
relative
intensities
of
these
masses
in
a
reference
mass
spectrum.
The
reference
mass
spectrum
can
be
obtained
from
a
standard
analyzed
in
the
HRGC/
MS
system
or
from
a
reference
library.

11.0
CALCULATION
11.1
Relative
response
factors
­
Analyze
each
instrument
performance
check
standard
and
spiked
adipose
tissue
sample.
Tabulate
the
area
response
of
the
characteristic
quantitation
ion
against
the
concentration
for
each
target
analyte
and
its
corresponding
internal
standard
(
Table
A­
2)
and
calculate
relative
response
factors
(
RRF)
using
Equation
1:
I
A­
I6
000113
Tentative
Identification
of
Major
Peaks
1.
Acetic
ucid
ethyl
ester/
Propanoic
acid
propyl
ester
2.
Heptanal
3.
Decane
4.
Dimethyfoctane
5.
Tr
imethylcyc
lohexane
6.
Nonanal
7.
Undecene
8.
Ethyl
ester,
­_
carboxylic
acid
9.
Nonadienal
Middle
Atlantic,
0­
14
years
4
3
ll
7
3:
2Y
Figure
A­
4.
HRGC/
MS
chromatogram
of
volatile
compounds
from
the
NHATS
FY82
composite
of
the
0­
14
yr
age
grou$
from
the
illddle
Atlantic
Census
Division.

A­
1
7
000114
Table
A­
2.
Characteristic
Ions,
Relative
Retention
Times
(
RRT),
and
Internal
Standards
Used
to
Quantitate
Target
Volatile
Organic
Analytes
Characteristic
quantitation
Compound
ion
(
m/
z)
RRT~

Bromochloropropane
Chloroform
d­
Ch1orof
orm
l,
l,
l­
Trichloroehtane
Bromodichloromethane
Benzene
d6­
Benzene
Tetrachloroethene
Dibromochloromethane
l,
l,
2­
Trichloroethane
To1
uene
dg­
Toluene
Chlorobenzene
d5­
Chlorobenzene
Ethy1benzene
dlo­
Ethylbenzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
d2­
1,1,2,2­
Tetrachloro
ethane
1,2­
Dichlorobenzene
de­
1,4­
Dichlorobenzene
1,4­
Dichlorobenzene
Xylene
dlo­
e­
Xylene
Ethylphenol
77
.
1.00
79
0.20­
0.43
82
0.20­
0.43
97
0.35­
0.58
129
0.53­
0.76
78
0.39­
0.62
84
0.39­
0.62
166
1.16­
3.39
129
1.05­
1.28
97
0.88­
1.11
91
0.83­
1.07
100
0.83­
1.07
112
.
1.48­
1.72
117
1.48­
1.72
106
1.62­
1.85
116
1.62­
1.85
173
1.79­
1.96
104
1.85­
2.08
83
2.05­
2.28
84
2.05­
2.28
146
2.88­
3.11
150
2.73­
2.96
146
2.73­
2.96
106
1.65­
1.88
116
1.65­
1.88
122
2.19­
2.43
Internal
standard
Bromochloropropane
d­
Chloroform
­
Bromochlororopane
Bromochloropropane
de­
Benzene
­.

Bromochloropropane
Bromochloropropane
Bromochloropropane
da­
Tol
uene
­*

d5­
Chlorobenzene
­
d
0
­
Ethy1benzene
­
Bromochloropropane
Bromochloropropane
d2­
1,1,2,2­
Tetrachloroethane
­

d4­
1,4­
Dichlorobenzene
­
d4­
1,4­
Dichlorobenzene
d
0­
E­
Xy
1ene
dlo­
thylbenzene
dlo­
FXylene
aRelative
retention
times
calculated
versus
the
internal
standard,
brornochloropropane
A­
18
000115
Equation
1.

=
area
of
the
characteristic
quantitation
ion
for
where:
As
the
target
analyte.

Ais
=
area
of
the
characteristic
quantitation
ion
for
the
internal
standard.

Cis
=
Concentration
of
the
internal
standard
(
pg).

Cs
=
Concentration
of
the
compound
to
be
measured.

If
the
RRF
value
over
the
working
range
is
a
constant
(<
40%
RSD),
the
RRF
can
be
assumed
to
be
invariant
and
the
average
RRF
can
be
used
for
calculations.
Alternatively,
the
results
can
be
used
to
plot
a
calibration
curve
of
response
ratios,
AS/
AiS
vs.
RRF.

11..
2
When
a
target
analyte
has
been
identified,
the
quantitation
of
that
compound
should
be
based
on
the
integrated
abundance
from
the
EICP
of
the
primary
quantitation
ion
given
in
Table
A­
2.

Calculate
the
concentration
in
the
sample
using
the
relative
response
factor
(
RRF)
determined
in
Section
11.1
and
Equation
2.

Equation
2.

Concentration
(
pg/
g)
=

where:
AS
=
area
of
the
character
stic
quantitation
ion
for
the
target
analyte.

Ais
=
area
of
the
characteristic
quantitation
ion
for
the
internal
standard.

Cis
=
concentration
of
the
corresponding
internal
standard
(
w>.

Wt
=
wet
tissue
weight
(
9).

12.0
REPORTING
12.1
Report
target
analyte
results
are
demonstrated
in
Figures
A­
5
and
A­
6.

12.2
Quantitative
data
must
be
qualified
to
provide
an
indication
of
the
intensity
of
response.
Quantitative
data
for
target
analytes
A­
19
m
f
m
..
U
f
3
0
ci
E
0
P
u
.
E.
m
X
w
W
L
3
0
A­
20,

000117
Report
Date:
Prepared
By:

Reviewed
By:

HUMAN
ADIPOSE
TISSUE
DATA
REPORTING
FORM
­
VOLATILE
ORGANICS
Census
Division
Composite
No.
Age
Group
Sample
Weight
Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Dibromochl
oromethane
'
1,1,2­
Trichloroethane
To1
uene
Chlorobenzene
Ethyl
benzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,
Z­
Di
chlorobenzene
1,4­
Dichlorobenzene
Xy
1ene
Ethy1pheno1
Total
pg/
Cornposite
Specimen
ES
­
East
South
Central
(
1)
(
1)
(
2)
(
1)
(
2)
0­
14
15­
44
15­
44
45+
45+
25.6
g
19.0
g
24.3
9
20.6
g
19.3
g
Figure
A­
6.
Example
data
report
format,
for
vofat.
iIe
organic
analytes
'

detected
in
composite
samples
from
a
specific
census
division.

A­
21
000118
13.0
responses
of
less
than
2.5
times
background
signal­
to­
noise
(
limit
of
detection,
LOD)
are
labeled
as
not
detected
(
ND).
Target
analyte
responses
ranging
from
2.5
to
10
times
the
background
signalto
noise
are
reported
as
trace
(
tr)
values.
Target
analytes
with
response
greater
than
10
times
the
background
signal­
to­
noise
(
limit
of
quantitation,
LOQ)
are
considered
positive
quantifiabie
(
PO)
values.

METHOD
PERFORMANCE
The
method
performance
as
determined
by
a
single
laboratory
for
instrument
performance
checks
and
spiked
adipose
tissue
specimens
are
presented
in
Tables
A­
3
and
A­
4.
These
data
were
generated
using
a
Finnigan
4000
quadrupole
mass
spectrometer
for
the
analysis
of
46
composite
specimens
from
the
National
Human
Adipose
Tissue
Survey
(
NHATS)
Fiscal
Year
1982
collection.
The
method
detection
limits
are
estimated
to
range
from
0.001
to
0.10
pg/
g
from
20­
9
tissue
samples
depending
on
the
specific
analyte
and
the
observed
interferences.

A­
22
008119
0
m
QI
v
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cum
drlm
m
0.010
w
mco
+
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n
nn­
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moo
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0
600
v
WWV
1.

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h
n
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0
c.
l
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v
n
cu
Y
Y
0
000
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vu
ow
u
ew
­
w
+
N
w
rl
m
hr
o
cy
m
*
c
ny
w.
cu
0
0
0
0
0
0
0
0
0
e
d
h
0
0
.­
d
W
A­
24
h
cn
h
hl
hl
0
v
dwh
o
r?
v
0
0.0
800121
I''
c
APPENDIX
B
VOLATILE
ORGANIC
COMPOUND
DATA
FROM
THE
NHATS
FY82
COMPOSITE
HUMAN
ADIPOSE
TISSUE
SAMPLES
B­
1
C,

8­
VI
U
C
3
0
a
E
0
.
u
U
V
.
C
c
m
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re)
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LW
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t­
v,
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c,
w
v
(
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wu
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a
0
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0
9
a
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0
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J
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m
c,
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W&
rcc
4.
r
w
El)

d­
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nri
.
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ri
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m
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+
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m
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id
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c,
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c
t
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3t­
I
vc,
0.
r
o.
:

V
B­
2
080123
Table
8­
2.
Summary
of
the
Total
Mass
(
pg)
of
Selected
Volatile
Organic
Compounds
Determined
in
the
Composited
Human
Adipose
Tissues
Representing
the
Mountain
(
MO)
Census
Division
Total
pg/
composi
te
specimena
Census
division
MO
­
Mountain
Composite
no.
(
1)
Age
group
0­
14
Sample
weight
5.1
g
Compound
Chloroform
0:
21b
1,
l,
1­
Trichloroethane
NO
(
1.2)
Bromodichloromethane
.
ND
(
2.3j
Benzene
(
1)
(
1)
15­
44
45+
18.8
g
22.4g
1.54
2.78
0.33
1.1
ND
(
1.0)
ND
(
1.2)
0.30
0.26
ND
(
0.07)
Tr,
0.10
ND
(
0.1)
ND
(
0.12)
NO
(
0.07)
NO
(
0.08)
0.28
0.55
0.12
0.090
0.40
0.66
ND
(
0.10)
NO
(
0.12)
1.8
1.7
ND
(
0.005)
ND,
(
0.009)
Tr,
0.015
Tr,
0.016
1.1
0.80
2.0
3.4
1.2
2.3
Tetrachloroethene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
l,
l,
Z,
Z­
Tetrachloroethane
I,
2­
Di
chlorobenzene
1,4­
Di~
hlorobenzene
0.49
ND
(
0.12)
ND
(
D.
12)
ND
(
0.23)
0.18
Tr,
0.011
0.12
ND
(
0.23)
1.8
ND
(
0.007)

E
ND
(
0.001)
0.091
Xylene
0.62
Ethy1pheno1
1.4
aData
for
chloroform,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol
,
1,1,2,2­
tetrachIoroethane
and
dichlorobenzene
calculated
by
i
so­
tope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
I
bND
=
Not
determined.
Value
in
parenthesis
represents
the
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
 
Two
responses
were
quantitated,
howver,
the
specif
ic
isomers
were
not
determined

8­
3
.

800124
,

Table
B­
3.
Summary
of
the
Total
Mass
of
Selected
Volatile
Organic
Compounds
Determined
in
the
Composited
Human
Adipose
Tissues
Representing
the
West
South
Central
(
WS)
Census
Division
Total
pg/
composi
te
specimena
Census
division
WS
­
West
South
Central
Composite
no.
(
1)
(
1)
(
2)
(
1)
Age
group
0­
14
15­
44
15­
44
45+
Sample
wei
ght
6.0
g
22.4
g
21.9
g
22.0
g
Compound
Chloroform
ND
(
0.60)
b
0.29
0.12
ND
(
0.74)
l,
l,
l­
Trichloroethane
5.0
ND
(
f.
6)
1.6
ND
(
1.9)
Bromodi
chl
oromethane
ND
(
3.0)
ND
(
3.2)
ND
(
1.8)
ND
(
3.7)
Benzene
ND
(
0.08)
0.31
0.067
0.51
Tetrachl
oroethene
ND
(
0.20)
ND
(
0.16)
0.35,
ND
(
0.19)
Dibromochloromethane
ND
(
0.20)
ND
(
0.16)
ND
(
0.08)
ND
(
0.19)
l,
I,
Z­
Trichlwoethane
ND
(
0.30)
ND
(
0.32)
ND
(
0.06)
ND
(
0.37)
To1uene
0.22
ND
(
0.004)
0.18
0.76
Chlorobenzene
0.015
0.063
0.031
0.19
Ethyl
benzene
,
1.7
5.6
1.4
,
3.7
Bromoform
ND
(
0.30)
ND
(
0.32)
ND
(
0.08)
ND
(
0.37)
...
Styrene
1.5
­
1.4
0.90
3.0
.
I,
l,
Z,
Z­
Tetrachloroethane
ND
(
0.01)
ND
(
0.03)
ND
(
0.008)
ND
(
0.03)
1,2­
Dichlorobenzene
ND
(
0.004)
Tr, 
0.037
ND
(
0.004)
Tr,
0.022
1,4­
Di~
hlorobenzene
2.
I.
2.6
11
4.3
Xylene
8.6
25
7.8
18
Ethy1pheno1
2.4
3.0
0.28
0.96
aData
for
chloroform,
benzene,
toluene,
chlorobenzene ,
ethyl
benzene,
xylene,
ethylphenol,
l,
l,
Z,
Z­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all.
cornpounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
Not
determined.
Value
in
parenthesis
represents
the
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
 
Two
responses
were
quantitated,
however,
the
specific
isomers
were
not
deter­

\
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ned.

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4
n
A
I
Q
a
c
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r
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9)
c,
W
n
c'
c,
L
w
c,
W
bct
O&

2.
E
m
E
4
v)
al
V
mnn
an
(
3
nn
L
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zz
z
zz
c,

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Q,
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c
rc
.

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vu
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no
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woo4orlo03oobmm
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.,
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kzzz
2%
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uw
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B­
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..
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.

Table
B­
6.
Summary
of
the
Total
Mass
of
Selected
Volatile
Organic
Compounds
Deterined
in
the
Composited
Human
Adipose
Tissues
Representing
the
West
North
Central
(
WN)
Census
Division
aTotal
pg/
composite
specimen
WN
­
West
North
Central
Census
division
Composite
no.
Age
group
Sample
weight
Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodi
chloromethane
Benzene
Tetrachl
oroethene
Di
bromochl
oromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Et
hy1benzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
(
1)
(
1)
0­
14
15­
44
18.9
g
21.6
g
ND
(
0.032a
0.31
ND
(
0.47)
ND
(
0.47)
ND
(
0.94)
ND
(
0.94)
0.090
0.34
0.51
'
0.39
ND
(
0.14)
ND
(
0.14)
ND
(
0.094)
ND
(
0.094)
0.15
0.40
.

0.020
0.020
0.32
0.99
ND
(
0.094)
NO
(
0.094)
0.30
0.61
(
1)
(
2)
45+
45+
21.6
g
18.3
g
0.15
'
0.23
0.58
ND
(
0.40)
ND
(
1.0)
ND
(
1.6)
0.10
0.12
0.79
'
0.'
58
ND
(
0.21)
ND
(
0.16)
ND
(
0.021)
ND
(
0.08)
0.13
0.055
0.020
0.032
0.16
0.53
ND
(
0.052)
ND
(
0.080)
0.18
0.55
ND
(
0.003)
ND
(
0.09)
0.040
ND
(
0.017)
1.1
0.301
0.59
1.5
Tr,
0.01
0.12
ND
(
0.001)
ND
(
0.001)
1,2­
Dichlorobenzene
Tr,
0.007
ND
(
0.010)
1,4­
Di~
hlorobenzene'
1.1
0.48
Xylene
1.5
1.7
Ethylpheno1
1.4
0.10
aData
for
chloroform,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
l,
l,
Z,
Z­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
Not
determined.
Value
in
parenthesis
represents
the
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quanti
tation
(
LOQ).
'
Two
responses
were
quantitated,
however,
the
specific
isomers
were
not
determined

0
0­
7
000128
W
U
E01
z
czz
E
W
t
W
 
0
coo
8
Pf
W
c,

0
YI
S
3
n
Ot
d
W
.
r
i
4
0)
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ci
E
0,

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y.
c
u
5:
al
&

h
L
I
m
>

W
W
c
B
0
c
c
W
f
Table
8­
8.
Summary
of
the
Total
Mass
of
Selected
Volatile
Organic
Compounds
Determined
in
the
Composited
Human
Adipose
Tissues
Representing
the
New
England
(
NE)
Census
Division
Total
pg/
composite
specimena
NE
­
New
England
Census
division
Composite
no.
Age
group
Sample
weight
Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichlorornethane
Benzene
Tetrachloroethene
Dibromochlorornethane
1,1,2­
Trichloroethane
To1uene
Chlorobenzene
Ethylbenzene
Bromof
orm
Styrene
1,1,2,2­
Tetrachloroethane
(
1)
0­
14
20.0
g
Try
0.070b
ND
(
0.44)
ND
(
2.2)
0.69
ND
(
0.08)
ND
(
0.22)
ND
(
0.22)
0.44
.
0.040
2.9
ND
(
0.22)
2.2
(
1)
15­
44
23.6
g
Tr,
,0.070
EJD
(
0.44)
ND
(
2.2)
.
0.58
ND
(
0.08)
ND
(
0.22)
ND
(
0.22)
1.0
0.10
1.7
ND
(
0.22)
4.1
C
C
8.2
0.91
(
1)
''
repeat"
(
1)
15­
44
45+
23.6
g
25.5
g
Tr,
0.060
0.16
0.39
ND
(
2.7)
ND
(
4.2)
ND
'(
5.4)
0.63
0.50
NO
(
0.15)
ND
(
0.80)
ND
(
0.42)
ND
(
0.50)
ND
(
0.42)
ND
(
0.50)
1.2
0.38
0.10
0.060
2.1
'
1.7
ND
(
0.42)
ND
(
0.30)
3.7
3.2
ND
(
0.030)
ND
(
0.020)
Tr,
0.020
ND
(
0.010)
2.6
0.30
11
9.7
4.2
3.9
ND
(
0.020)
1,2­
Dichlorobenzene'
Tr,
0.019
1,4­
Di~
hlorobenzene
0.45
Xylene
3.8
Ethylphenol
2.3
aData
for
chlorororm,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
1,1,2,2­
tetrachloroethane
and
dichlorobenzene
calcu1,
atedby
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
Not
determined.
Value
in
parenthesis
represents
the
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
'
The
HRGC/
MS
program
was
interrupted
before
the
analysis
was
completed.
dTwo
responses
were
quantitated,
however,
the
specific
isomers
were
not
determined.

B­
9
000130
I
..

fable
B­
9.
Summary
of
the
Total
Mass
of
Selected
Volatile
Organic
Compounds
Determined
in
the
Cornposited
Human
Adipose
Tissues
Representing
the
Pacific
(
PA)
Census
Division
Total
pg/
cornposite
specimena
PA
­
Pacific
Census
division
Composite
no.
Age
group
Sample
weight
(
1)
0­
14
15.0
g
(
1)
15­
44
17.4
g
(
1)
45+
20.7
g
Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
1.1
4.2
0.14
ND
(
0.80)
Tr,
0.10
1.8
ND
(
2.3)
0.22
Tr,
0.050
NO
(
0.30)
ND
(
1.1)
0.17
Tetrachloroethene
Di
bromochloromethane
1,1,2­
Trichloroethane
To1uene
NO
(
0.060)
ND
(
0.050)
ND
(
0.30)
0.17
0.19
ND
(
0.23)
ND
(
0.23)
0.34
Try
0.11
ND
(
0.11)
ND
(
0.11)
0.26.
Chlorobenzene
0.030
0.040
0.020
Ethylbenzene
Bromoform
Styrene
1,1,2,2­.?
etrachloroethane
I,
2­
Dichlorobenzene
1,4­
Di~
hlorobenzene
Xylene
Ethy1pheno1
ND
(
0.040)
ND
(
0.30)

ND
(
0.010)
Tr,
0.009
1.7
0.35
0.72
0.75
0.68
NO
(
0.23)
2.5
ND
(
0.020)
0.073
0.29
0.81
0.55
0.58
ND
(
0.11)
1.0
ND
(
0.010)
Tr,
0.011
0.30
0.62
0.35
­__

for
chloroform,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
1,1,
ZY2­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol'where
deuterated
ethylbenzene
was
used,
were
available'as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
Not
determined.
Value
in
parenthesis
represents
the
estimated
.
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
'
Two
responses
were
quantitated,
however,
the
specific
isomers
were
not
deter
mined.

B­
10
BOO131
Table
B­
10.
Summary
of
the
Concentration
(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipos!
Tissue
Specimens
Representing
the
East
South
Central
(
ES)
Census
Division
Census
division
ES
­
East
South
Central
Composite
no,
Age
group
I
(
1)
0­
14
(
1)
(
2)
(
1)
15­
44
'
15­
44
45+
(
2)
45+

Compounda
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
ND
(
11)
Tr,
3.6
ND
(
10)
ND
(
28)
66
ND
(
21)
ND
(
28)
NO
(
74)
ND
(
21)
7.9
4.0
8.3
ND
(
10)
100
ND
(
73)
.
2.6
Tetrachloroethene
29
Tr,
4.6
ND
(
3)
12
Dibromochloromethane
ND
(
3)
ND
(
3)
ND
(
2)
ND
(
6)
I,
l,
Z­
Trichloroethane
ND
(
6)
ND
(
2)
ND
(
5)
ND
(
4)

~

Toluene
18
7.6
16
2.5
Chlorobenzene
1.7
3.9
2.6
1.6
Ethylbenzene
9.0
12.1
13
16
Bromoform
ND
(
8)
ND
(
3)
ND
(
8)
ND
(
6)
Styrene
79
.28.4
46
46
1,1,2,2­
Tetrachloroethane
ND
(
0.2)
2.1
ND
(
0.3)
8.0
1,2­
Dichlorobenzene
ND
(
0.1)
Tr,
0.7
Tr,
0.2
Tr,
0.3
.
1,4*
DifhIorobenzene
40
49
300
320
Xylene
56
55
57
60
Ethylpheno?
17
8
40
29
.~,

,
>:.
'.
,
aData
for,
chloroform,'
ben.
zene:
to1uene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol',
1,
l,
Z,
Z­$
etrachloroe)
hane
,
and'di.
chl,
orobenzene
calculated
by
i
so­

!"
tope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of,

,­.',_
ethylphenof
where
deuterated
:
ethylbenzenewas
usqd,
were
,
avai1ab1e
as
interna
standards.
AI
1
ot$
er
'
compoundswere
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
.:,
bhD
­­
not
detected.
Value
in
.
par,
enthesissignifies
an
estjhated
detection
.
limit.
Tr
signifies
trace
level
between
li'mit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
'
Two
respohses
were.
quantitated,
however,
the
'
spec:
fic
i
somers
were
not
determined

B­
11
000132
Table
6­
11.
Summary
of
the
Concentration
'(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipose
Tissue
Specimens
Representing
the
Mountain
(
MO)
Census
Division
Census
division
Composite
no.
Age
group
1.

Compounda
Chloroform
l,
l,
l­
Trichloroethane
Brornod
ich
1
oromethane
Benzene
Tetrachloroethene
D
i
bromochloromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Ethy1
benzene
Bromoform
5
tyrene
1,1,2,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1,4­
Di~
hlorobenzene
Xylene
Ethylphenol
MO
­
Mountain
(
1)
(
1)
(
1)
0­
14
15­
44
45+

41
b
82
120
ND
(
240)
18
49
ND
(
450)
ND
(
53)
ND
(
50)
97
20
12
ND
(
24)
ND
(
4)
Tr,
5
.

NO
ND
(
45)
35
ND
(
4)
15
ND
(
4)
25
Tr,
2.2
6.4
4.0
24
21
30
ND
(
45)
353
ND
(
5)
96
ND
(
5)
76
ND
(
2)
ND
(
0.2)
18
ND
(
0.3)
Tr,
0.8
59
ND
(
0.4)
Try
0.7
36
120
110
150
(
24)
ND
(
5)
ND
(
41
270
64
100
aData
for
chloroform,
benzene,
to1uene
chl
orobenzene
,
ethyl
benzene,
xylene
ethylphenol,
1,1,2,
Z!­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compbunds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
not
detected.
Value
in
parenthesis
signifies
an
estimated
detection
*

4limit,
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quhntitation
(
LOQ).
'
Two
responses
were
quantitated,
however
the
specific
isomers
were
not
determined

B­
12
000133
Table
6­
12.
Summary
of
the
Concentration
(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipose
Tissue
Specimens
Representing
the
West
South
Center
(
WS)
Census
Division
Census
division
Composite
no.
Age
group
Compounda
Chloroform
1,1,
l­
Tri
chloroethane
Bromodichloromethane
Benzene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1.4­
Di~
hlorobenzene
Xylene
Ethylphenol
a
Data
for
chloroform,
benzene,
WS
­
West
South
Central
(
1)
(
1)
(
2)
(
1)
0­
14
15­
44
15­
44
45+

ND
13
5.3
ND
(
34)
a30
ND
(
71)
75
ND
(
84)
ND
(
500)
ND
(
140)
NO
(
82)
ND
(
170)
ND
(
13)
14
3.1
23
ND
(
33)
ND
(
7)
ND
(
4)
NQ
(
9)
ND
(
SO)
ND
(
14)
ND
(
3)
ND
(
17)
37
NO
(
0.2)
8.4
35
2.5
3.0
1.4
8.6
280
250
64
168
ND
(
SO)
ND
(
14)
ND
(
4)
ND
(
17)
250
63
41
136
(
2)
ND
(
1)
ND
(
0.4)
ND
(
1..
4)
ND
(
0.7)
Tr,
1.7
ND
(
0.2)
Tr,
1.0
350
120'
500
200
k
,400
1,100
360
810
400
140
13
44
~
~~

toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
1,1,2,2­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ettiylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
A1
1
'
other
compounds
were
quantitated
versus
the
internal
standard
bromochl
oropropane
(
BCP).
bND
=
not
detected.
Value
signifies
an
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
'
Two
responses
were
quantitated,
however,
the
specific
isomers
were
not
deter­
mi
ned.

,

 3­
13
000134
TI­
I
a
w
w
c,
.

Iv
0
P
­+
V
Nu,
Ub
C
.
r
n+

­*

CaJ
c
mr
mc,

e
nd
dl
wo
m
d
I
m
c
0
aJ
'
C
.
P
a
m
+
n
nn
Ah
n
n
0
OO
a
nL
z
zz
z
zc
on
onc,
n
I­
Lzz
zzz
z
­'
>,
ZUJT
v
cc,
maL
0
­
IC
hW0
c
mmr
c,
c
0
m
c,.
C
0
wc,
I
B­
14
000135
Table
8­
14.
Summary
of
the
Concentration
(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipose
Tissue
Specimens
Representing
the
Middle
Atlantic
(
MA)
Census
Division
Census
division
MA
­
Middle
Atlantic
Composite
no.
(
1)
(
2)
(
1)
(
2)
(
1)
(
1)
Age
group
0­
14
0­
14
15­
44
15­
44
45+
45+

Compounda
Chloroform
.
6.4b
7.7
6.4
79
14
Tr,
5..
6
1,1,1­
7ric
hloroethane.
ND
(
17)
NO
(
19)
97
30
ND
(
28)
ND
(
30)
Bromodichloromethane
ND
(
37)
ND
(
39)
NO
(
40)
ND
(
91)
ND
(
61)
ND
(
100)
Benzene
6.4
11
8
25
­
13
15
Tetrachloroethene
49
16
75
30
94
46
Dibromochlorornethane
ND
(
io)
ND
(
4)
ND
(
10)
ND
(
9)
ND
(
15)
ND
(
IO)
l,
l,
Z­
Trichloroethane
ND
(
5)
NO
(
3)
ND
(
6)
NO
(
5)
ND
(
9)
ND
(
5)
Toluene
4.4
Tr,
0.7
6.8
9.1
14
ND
(
0.2)
Chlorobenzene
2.0
0.6
2.4
6.7
3
2.5
Ethylbenzene
8.4
6.6
14
12
14
0.1
Bromoform
ND
(
5)
ND
(
4)
ND
(
6)
ND
(
8)
ND
(
9)
ND
(
8)
Styrene
41
44
39
39
45
42
1,1,2,2­
Tetrachloroethane
ND
(
0.3)
ND
(
0.4)
ND
(
0.4)
ND
(
0.4)
ND
(
1)
ND
(
0.6)
1,2­
Dichlorobenzene
Tr,
1.4
Tr,
,
0.3,
Tr,
1.1
Tr,
1.4
Try
1.4
Tr,
0.8
1,4­
Di$
hlorobenzene
30
.
24
18
320
59
220
Xylene
19
28
57
52
54
41
Ethylphenol
21
47
66
68
120
31
a
Data
for,
chloroform,
benzene,
toluene,
chlorgbenzene,
ethylbenzene,
xylene,
ethylphenol,
l,
l,
Z,
Z­
tetrachloroethane,
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
not
detected.
Value
in
parenthesis
signifi'es
an
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
'
Two
responses
were
quantitated,
however,
the
specific
isomers
were
not
determined.

B­
15
000136
I
Table
B­
15.
Summary
of
the
Concentration
(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipose
Tissue
'
Specimens
Representing
the
West
North
Central
(
WN)
Census
Division
~

Census
division
WN
­
West
North
Central
Compos
i
te
no.
(
1)
(
1)
(
2)
(
2)
.
Age
group
.
0­
14
15­
44
45+
45+

Compounda
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
ND
(
2)
b
ND
(
24)
ND
(
50)
4.8
14
ND
(
22)
ND
(
43)
16
7.0
27
ND
(
48)
4.6
13
ND
(
22)
ND
(
87)
6.5
Tetrach
1
oroethene
27
18
37
32
Dibromochloromethane
1,1,2­
Trichloroethane
To1uene
ND
(
7)
ND
(
5)
8.0
ND
(
7)
ND
(
4)
19
ND
(
0.9)
NO
(
1)
6
ND
(
9)
ND
(
4)
3
Chlorobenzene
1.1
0.9
0.9
1.7
Ethy1
benzene
17
'
46
7.4
29­
Bromoform
ND
(
5)
ND
(
4)
ND
(
2)
ND
(
4)
Styrene
16
28
8
30
1,1,2,2­
Tetrachloroethane
ND
(
0.1)
ND
(
0.1)
ND
(
0.1)
ND
(
5)
1,2­
Dichlorobenzene
Tr,
0.4
ND
(
0.5)
1.9
ND
(
0.4)
1,4­
Di$
lorobenzene
.
.58
22
51
16
Xylene
79
81
27
81
Ethylphenol
72
5
Tr,
0.4
7
a
Data
for
chloroform,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
l,
l,
Z,
Z­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
not
detected.
Value
in
parenthesi's
signifies
an
estimated
detection
limit.
Tr
signifies
trace
level
between
'
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
CTwo
responses
were
quantitated,
however,
the
specific
isomers
were
not
determi
ned.

6­
16
000137
c,
.
.
I
',
P
...;..­.
._
1
.,.
.
I.

/'
'

nd
u
VI
U'I
3
VI
n
nne
=
3':
aJ
r
.­
an0
on
n
on
v)
zzz
zz
z
zz
0
Q)
>
w
u
da
7
CC
Q)

U.­
0
a
on
o
nc,
m
.
P
z
zz
z
zz
L
­
c,
n
n
cn
Q,
.
C
W
v
VU
'
4
0
00
0
z
zz
e,

0,
L
at
3
0)
L
al
E
0
v)
­
c
'
E
u
m
.
C
.

u
nd
NI
­
0
n
nnno
0
OL
'
z
zzzz
z
zt
d
nrl
rll
uo
on
non
n
nnzz
zzz
z
fZ
lD
rl
I
m
owe
LCCat
oww
7
n
m
t
B­
17
000138
Table
B­
17.
Summary
of
the
Concentration
(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipose
Tissue
Specimens
t
Representing
the
Pacific
(
PA)
Census
Division
Census
division
Composi
te
no.
Age
group
Compounda
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
6enzene
Tetrachloroethene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To
1uene
Chlorobenzene
Ethy1benzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1.4­
Di~
hlorobenzene
Xylene
Ethylphenol
PA
­
Pacific
(
1)
(
1)
(
1)
0­
14
15­
44
45+

75
Try
5.7
Tr,
2.4b
280
100
NO
(
14)
NO.
(
53)
ND
(
130)
ND
(
53)
9.0
13
8.2,
ND
(
4)
11
Tr,
5.5
ND
(
3)
ND
(
13)
ND
(
5)
ND
(
20)
ND
(
13)
ND
(
5)
11
20
13
2
.
2.3
 
1.0
NO
(
3)
39
28
ND
(
20)
ND
(
13)
ND
.(
5)
50
140
50
ND
Tr,
0.6
4.2
Tr,
0.5
110
17
15
24
 
46
30
48
32
.
17
(
0.7)
ND
(
1)
ND
(
0.5)

~
­~

aData
for
chloroform,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
1,1,2,2­
tetrachloroethane
and
dichlorobenzene
calculated
by
isotope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
available
as
internal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
bND
=
not
detected.
Value
in
parenthesis
signifies
an
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOD)
and
limit
of
quantitation
(
LOQ).
 
Two
responses
were
quantitated,
however,
the
specific
isomers
were
not
de
termined.

6­
18
OQQ139
5
Table
B­
18.
Summary
of
the
Concentration
(
ng/
g)
of
Target
Volatile
Organic
Compounds
in
Composite
Human
Adipose
Tissue
Specimens
Representing
the
New
England
(
NE)
Census
Division
Census
division
NE
­
New
England
Composi
te
no.
(
1)
b
(
1)
(
1)
Age
group
0­
14
15­
44
15­
44
45+
(
repeat)
...
,

Chloroform
Tr,
3.5c
Try
3
Tr,
2.5
6.3
l,
l,
l­
Trichloroethane
ND
(
22)
ND
(
19)
17,
ND
(
110)
Bromodichloromethane
ND
(
110)
ND
(
93)
ND
(
180)
NQ
(
310)
Benzene
59
25
27
20
Tetrachloroethane
ND
(
4)
ND
13)
ND
(
6)
ND
(
31)
Dibromochloromethane
ND
(
14)
ND
(
9)
ND
(
18)
ND
(
20)
l,
l,
Z­
Trichloroethane
ND
(
11)
ND
(
9).
ND
(
18)
ND
(
20)
To1uene
22
42
51
15
Chlorobenzene
2
4.2
40
Ethylbenzene
145
72
89
67
Bromoform
ND
.
(
11)
ND
(
9)
ND
(
18)
ND
(
12)
Styrene
110
170
160
124
1,1,2,2­
Tetrachloroethane
ND
(
1)
b
ND
(
1)
ND
(
0.8)
1,2­
Dichlorobenzene
Tr,
1.0
b
Tr.
1
ND
(
0.4)
1,4­
Di~
t~
lorobenzene
148
358
it88
383
&?$?
E
heno1
120.
38
180
150
aData
for
chloroform,
benzene,
toluene,
chlorobenzene,
ethylbenzene,
xylene,
ethylphenol,
1,1,2,2­
tetrachforoethane
and
dichlorobenzene
calculated
by
iso
tope
dilution.
Deuterated
analogs
of
all
compounds,
with
the
exception
of
ethylphenol
where
deuterated
ethylbenzene
was
used,
were
availab1e
as
in
ternal
standards.
All
other
compounds
were
quantitated
versus
the
internal
standard
bromochloropropane
(
BCP).
PThe
HRGC/
MS
analysis
was
interrupted
before
the
sample
analysis
was
completed.
'
ND
=
not
detected.
Value
in
parenthesis
signifies
an
estimated
detection
limit.
Tr
signifies
trace
level
between
limit
of
detection
(
LOG)
and
limit
of
quantitation
(
LOQ).
dTwo
responses
were
quantitated,
however,
the
specific
isomers
were
not
de
termined.

6­
1
9
000140
2.4
APPENDIX
C
COMPOSITING
SCHEME
FOR
THE
NHATS
FY82
SPECIMENS
c­ 
1
000141
COMPOSITING
SCHEME
The
NHATS
FY82
specimens
were
composited
according
to
a
scheme
provided
by
the
OTS
Design
and
Development
Branch
(
DDB)
prime
contractor,
Battelle
Columbus
Laboratories
(
BCL).
The
following
tables
provide
the
details
of
the
actual
compositing
effort.
Composites
for
semivolatile
organic
analysis
were
completed
first.
Thus.,
many
of
the
specimens
identified
by.
BCL
were'depleted
before
the
volatile
composite
was
prepared.

The
aliquot
for
each
individual
specimen
added
to
the
composites
is
specified
and
the
approximate
mass
of
each
individual
specimen
remaining
after
compositing
is
listed..
Most
samples
contain
up
to
20
g
total
adipose
tissue.
However,
two
samples
(
WS
­
Composite
1,
0­
14
yr
and
MO
­
Composite
1,
0­
14
yr)
consist
of
only
5­
10
g
total.
This
is
a
result
of
the
very
small
sample
sizes
that
were
available.
Many
of
the
samples.
for
the
MO
census
division
could
not
be
located
in
the
repository.
The
notation,
NS,
indicates
no
sample
was
found.

One
error
in
the
actual
compositing
should
be
noted.
Sample
8202780
was
included
in
the
WS
Composite
1,
45
plus
sample
instead
of
the
15­
44
cornposite
as
specified
in
the
BCL
plan.

c­
2
000142
I.
.
.
...

Census
Division
=
PA,
Age
Group
=
0­
14
Years,
Composite
1
Semivolatile
Volati
12
Approximate
FY
82
organic
composite
organic
composite
mass
specimen
no.
amount
added
(
9)
amount
added
(
9)
remaining
(
9)
b.

8206310
3.1
0.8
0
8206336
2.9
3.2
3
8206344
2.4
0
0
8206351
2.8
3.2
1.0
8206294
2.7
2.9
1.5
8206328
2.9
2.3
.
0
8206369
2.9
2.6
­­
0
..

Total
composite
(
9)
19.7
15.0
Date
composited:
2/
27/
84
c­
3
000143
Census
Division
=
PA,
Age
Gro'up
=
15­
44
Years,
Composite
1
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
Vol
ati1
e
organic
cornposit­
e
'
amount
added
(
9)
Approximate
mass
remaining
(
9)

8206153
8206195
8206229
2.2
2.6
2.
a
2.2
2.2
2.2
4
4
4
8206419
8206211
8206237
2.4
2.2
2.3
2.6
1.1
2.3
.3
2
4
8206245
8206260
2.3
2.6
2.2
2.6
3
4
8206203
2.2
0
­­
0
Total
composite
(
9)
21.6
17.4
Oate
composited:
2/
27/
84
c­
4
000144
.
I
Census
Division
=
PA,
Age
Group
=
45
+
Years,
Composite
1
Semi
vol
at:
?
e
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8206278
1.3
8206286
1.3
8206302
1.1
8206435
1.8
8205346
1.9
.
8205353
1.6
8205361
1.7
8206252
1.5
8206377
1.2
,

8206385
1.2
8206393
1.4
8205387
1.2
8206401
1.8
8206427
1.4
8206443
1.6
­
Total
composite
(
9)
22.0
Date
composited:
2/
27/
84
V3
1at
S
1e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.3
25
1.5
10
1.7
15
1.3
20
I.
3
10
1.1.
5
1.5
.5
1.4
20
1.4
15
1.2
10
1.8
15
1.6
15
1.3
10
0.9
25
1.4
10
­
20.7
c­
5
000145
Census
'
Division
=
NE,
Age
Group
=
0­
14
Years,
Composite
1
Semivolati
1e
Vol
at?
1e
Approximate
FY
82
specimen
no.
organic
composite
amount
added
(
9)
organic
composite
amount
added
(
9)
mass
remaining
(
9)

8110678
8110686
8110710
8110736
8110744
8110751
8111072
8303737
8303794
8110975
8111007
8111015
8111049
8111098
8303778
8303711
'
8303919
0.8
0.9
0.9
1.5
1.3
1.4
1.
I
NS
0.9
1.4
1.2
1.2
1.2
1.4
1.2
1.5
1.2­
1.5
1.1
1.6
1.4
1.2
0.5
1.2
NS
1.2
0.9
1.4
1.4
1.0
1.1
1.3
1.9
1.3­
3
1
3
3
0
1
NS
0.5
3
5
7
4
1
4
3
7
<
O
20.0
Total
composite
(
9)
19.1
Date
composited:
2/
27/
84
C­
6
000146
Census
Division
=
NE,
Age
Group
='
15­
44
Years,
Composite
1
FY
82
specimen
no.

8110660
8110728
8110769
8110777
8110785
.
8110793
8110801
8303661
8303679
8303687
8303729
8303810
8303927
8110827
8110983
8110991
8111031
8111056
8111064
8111080
8303802
8303851
8110702
8303893
Semi
vo
1r?
t
i
le'
organic
composite
amount
added
(
9)
,
Volatile
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

1.0
1.0
5
1.0
1.2
3
1.0
1.0
4
1.1
1.0
4
1.0
1.0
'
4.
1.1
1.3
5
1.1
1.1
2
1.0
1.0
2
1.1
1.1
3
1.1
1.1
3
NS
NS
NS
1.0
1.0
2
1.0
1.1
5
1.1
1.7
1
1.0
1.0
2
1.2
1.0
2
1.1
1.1
2
1.2
1.1
2
0.8
1.3
2
1.0
1.1
2
1.0
1.2
3
NS
NS
NS
1.0
1.2
2
NS
NS
NS
­
7
Total
composite
(
9)
21.9
23.6
Date
composited:
2/
27/
84
c­
7
080147
I
Census
Division
=
NE,
Age
Group
=
45
+
Years,
Composite
1
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8110819
1.2
8110835
1.3
8110843
1.2
8110876
1.3
8110884 
1.3
8110934
1.8
8110959
2.0
8111023
1.1
8303752
NS
8303828
1.2
8303877
NS
8110694
1.2
8110850
1.0
8110868
1.2
8110892
2.2
8110900
1.5
8110918
1.6
8110926
2.2
8110942
1.1
8110967
1.3
8303836
1.0
­

Total
composite
(
9)
26.7
Date
composited:
2/
27/
84
Vo
7
at
i
1e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.0
3
I.
5
5
1.3
3
1.3
5
1.5
4
.
1.4
5
1.6
3
1.0
7
NS
NS
1.0
6
NS
NS
1.6
7
.
1.3
1
1.8
3
1.0
6
1.2
3
1.6
2.5
1.9
2
1.4
6
1.3
0
0.8
2
­
25.5
C­
8
000148
Census
Division
=
MA,
Age
Group
=
0­
14
Years,
Composite
1
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
Ppproximate
mass
remaining
(
9)

8205023
0.7
0
8205031
0.9
0
8205049
0.5
0
8201790
2.5
25
8201808
2.7
20
8206062
2.8
20
8206088
3.0
20
8206187
3.0
25
a201485
2.8
20
8206021
3.
I
20
a110595
NS
NS
8110652
NS
NS
8205007
1.0
0
8300006
NS­
US
Total
composite
(
9)
23.0
Date
composited:
2/
28/
84
Vo
1ati
1
e
organic
composite
amount
added
(
9)

0
0
0
3.0
3.0
2.6
3'.
I
3.0
2.6
3.0
NS
NS
0
NS
­
20.3
c
c­
9
000149
Census
Division
=
MA,
Age
Group
=
15­
44
Years,
Composite
I
Semivolatile
fY
82
organic
composite
specimen
no.
amount
added
(
9)

­

8201584
8201659
8205965
8205999
8206013
8203143
8203176
8203358
8203366
8203374
8201642
8201832
8205817
8205833
8205841
8205882
8206161
8203168
8203226
8203325
8205973
8203408
8201543
8205858
Total
composite
(
9)
1.0
1.1
1.1
1.1
1.0
I.
0
1.0
1.1
1..
o
1.0
1.0
0.9
1.0
1.2
0.9
1.1
1.0
1.1
1.2
1.0
1.1
1.0,
1.1
1.2
­
25.2
Vol
ati
:
s
Approxi­
mate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.1
10
1.2
10
1.0
5
1.2
5
1.1
10
0.7
3
1.0
5
1.2
10
1.4
.
5
1.1
10
1.1
10
1.0'
10
1.1
10
1.2
10
0.9
5
1.1
10
0.9
10
1.0
10
I.
0
5
1.0
10
1.1
10
0.4
2
1.2
2
1.0
.5
­
25.0
Date
composited:
2/
28/
84
c­
10
000150
Census
Division
=
MA,
Age
Group
=
45
+
Years,
Composite
1
Semivolatile
Volatile
Approximate
FY
a2
specimen
no.
organic
composite
amount
added
(
9)
organic
composite
amount
added
(
9)
mass
remai
ni
ng
(
9)

8201469
0.7
0.7
20
a201501
0.9
1.0
25
8201576
0.9
0.9
15
8201675
0.6
1.0
2.5
8201717
0.9
0.7
25
8201782
1.0
0.9
20
azo3135
0.9
0.8
'
20
azo3184
0.7
0.7
15
8203291
0.9
0.8
20
8203341
0.8
0.9
25
8300584
NS
NS
NS
a201451
0.8
0.7
25
8201519
0.8
1.0
25
8201535
0.9
0.9
20
8201600
0.7
0.7
25
801667
0.7
0.8
25
a203192
0.7
0.
a
20
8203317
0.7
0.
a
25
8300600
NS
NS
NS
8300618
NS
NS
NS
a300642
NS
NS
NS.
8207185
1.0
0.
a
15
azoiai6
0.
a
0.6
25
8300444
NS
NS
NS
8201447
0.
a
0.8
­­

Total
composite
(
9)
16.2
16.3
Date
cornposited:
2/
28/
84
e­
11
Census
Division
=
MA,
Age
Group
=
0­
14
Years,
Composite
2
FY
82
specimen
no.

8300030
8201550
8201691
8206104
8206112
8206120
8206179
8206005
8206039
8206047
8206054
8205056
8206070
8201626
Total
composite
Date
composited:
Semivolatile
organic
composite
amount
added
(
9)

NS
1.6
1.4
1.3
1.5
1.4
1.2
1.2
2.4
1:
s
1.7
1.1
2.5
.
I.­
4
20.2
2/
29/
84
Vol
ati
1e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

NS
NS
1.6
15
1.5
25
1.5
20
1.3
20
1­
5
20
1.2
10
1.2
20
1.7
20
1.4
25
2.3
15
0
0
1.4
20
­
1.5
25
18.1
­.

c­
12
000152
Census
Division
=
MA,
Age
Group
=
15­
44
Years,
Composite
2
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8201634
1.3
8201824
1.1
8205890
1.6
8205916
1.3
8205924
1.1
8205932
1.4
8205940
1.1
8205957
1.2
8205981
1.3
8203267
0.6
8205791
1.2
'
8205825
1.1
8205866
1.5
8205874
1.2
8206146
1.2
8203127
1.1
8203218
1.0
8203234
1.0
8203333
1.6
8201840
1.1
8203283
1.0
8206138
1.1­
Total
composite
(
9)
26.1
Date
composited:
2/
29/
84
i'

i
Vo
1ati
1
e
Apprcximat2
organic
composite
I
mass
amount
added
(
9)
remai
ni
ng
(
9)

1.2
10
1.1
10
1.2
10
1.6
10
1.2
10
1.1
10
1.3
10
1.0
10
1.4
10
0.6
5
1.0
10
1.3
10
1.2
10
1.3
LO
1.0
LO
0.9
5
1.0
10
1.0
10
.
1.2
8
1.2
10
1.0
5
­
10
1.5
25.3
c­
13
000153
Census
Division
=
MA,
Age
Group
=
45
+
Years,
Composite
2
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
Volatile
organic
composite
amount
added
(
9)
Approxi
mate
mass
remaini
ng
(
9)
..

8201493
8201568
8201592
8201709
8201725
8201774
8203150
8203259
8300451
8300485
8201618
8201733
8201758
8201766
8201857
8203200
8203275
8203382
8203424
8300568
8300634
8201527
8201683
8203309
8300659
0.8
0.8
0.7
0.8
0.7
0.8
0.8
0.8
NS
NS
1.2
0.7
1.2
1.3
1.4
0.9
0.8
0.9
0.8
NS
NS
NS
0.9
1.0
0.7­
0.8
0.8
0.8
0.9
1.0
1.0
0.7
0.7
NS
NS
0.8
0.7
1.1
1.0
0.6
1.0
0.7
1.2
0.9
"
S
NS
NS
0.9
1.4
0.8­
20
25
25
25
25
20
25
15
NS
'

NS
20
25
25
25
20
20
'

20
20
20
NS
NS­
NS
20
25
25
17.8
Total
composite
(
9)
18.0
Date
composited:
3/
1/
84
C­
14
..

L
Census
FY
82
specimen
no.

8201246
8203101
8207979
8206864
8206930
8200065
8200230
8200354
8201360
8203077
8203119
8200214
8203416
8210189
8210247
82030IO
8203465
8210205
8210403
8210379
Division
=
EN,
Age
Group
=
0­
14
Years,
Composite
1
Semivalati
le
organic
composite
amount
added
(
9)
Vol
ati
7
e
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

1.3
1.4
5
1.0
0
0
1.5
1.1
1
I.
0
1.2
5
1.2
1.2
5
0.8
0
0
0.6
0
0
0.5
0
.
o
1.1
1.1
2
1.4
0.8
0
1.0
1.0
1
1.0
1.2
0
1.0
0.5
0
1.0
.
1.5
0.5
NS
NS
NS
1.2
0.9
2
0.8
0
0
NS
NS
NS
0.9
0.8
­
1
0.8­
0­
0
12.7
Total
composite
(
9)
18.1
Date
composi
ted:
2128/
84
C­
15
000155
Census
Division
='
EN,
&
ge
Group
=
15­
44
Years,
Composite
1
Semivolatile
FY
a2
organic
composite
specimen
no.
amount
added
(
9)

~

__
~

8201162
0.8
8201170
1.2
8201188
1.0
8201238
0.9
8201345
0.9
8203630
0.9
8205288
1.3
8200297
1.1
8210171
0.9
8201352
1.2
8201386
1.1
8201436
0.8
8203028
2.2
8205163
0.8
8200370
'
1.0
8200388
0.8
8203432
0.9
8203499
1.3
8210346
NS
8200081
1.2
8210270
1.3
­

Total
composite
(
g)
21.6
Date
composited:
,2/
28/
84
Volatile
Approximate
organic
composite
mass
amount
added
(
9)
remai
ni
ng
(
9)

0.9
5
1.1
10
0.9
5
0.9
10
1.1
15
1.1
5.
0.9
2
1.4
2
1.
I
5
0.9
10
1.4
10
1.
I
15
3.3
2
0.7
10
0.8
0
1.0
3
0.8
10
0.5
0
NS
NS
0
0
0.9
­
4
20.8
C­
16
000156
Census
Division
=
EN,
Age
Group
=
45
+
Years,
Composite
1
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8201287
1.2
8201378
1.1
8201410
1.4
8203051
1.1
8205148
1.0
8200313
*
1.1
8200487
1.0
8200503
1.3
8207201
1.0
8201212
1.1
8205175
1.
I
8205320
1.0
8200438
1.0
8200453
1.3
8200461
1.0
8210148
NS
8210353
1.0
8207243
1.0
8210320
1.1
Total
composite
(
g)
19.8
Date
composited:
2/
28/
84
Vol
eti
?
e
Approx
i
mate
organic
composite
mass
amount
added
(
9)
remai
ni
ng
(
g)

1.1
10
1.1
5
1.2
5
1.2
5
1.0
2
1.1
10
1.4
.2
1.0
2
1.0
5
1.0
5
1.1
5
1.1
5
1.0
1
1.0
2
1.0
2
NS
NS
0.1
0
1.1
.
10
­.
2
1.1
18.6
c­
I
7
Census
Division
=
EN,
Age
Group
=
0­
14
Years,
Composite
2
FY
82
specimen
no.
Semi
vol
ati1e
organic
composite
amount
added
(
9)
Vol
ati
7
e
organic
composite
amount
added.
(
9)
Approximate
mass
remai
ni
ng
(
9)

8207961
1.5
1.4
2
8206922
1.0
1.1
4
8205304
0.9
0
0
8203085
1.8
2.0
0
8207953
1.1
1.0
5
8206880
1.2
'
1.2
1
8206856
1.1
1.6
2
'
8206872
1.2
0.6
1'
8200396
1.1
0.3
0
8203440
1.1
1.1
1
8210221
0.2
0
0
8206914
1.0
0.9
4
8200040
1.1
0
0
8200404
0.9
1
1
8210254
0.9
0
0
8210288
NS
NS
NS
8210411
1.1
1.2
1
8203036
1.1
1.2
1'
8203069
0.6
0.8
1
8200412
1.3
1.0
5
8203457
1.0­
0.9­
1
17.3
Total
composite
(
9)
21.2
Date
composi
ted:
3/
1/
84
C­
18
000158
Census
Oivision
=
EN,
Age
Group
=
15­
44
Years,
Composite
2
Semivolatile
FY
82
organic
composite
specimen
nu.
amount
added
(
9)

8201204
1.1
8201311
1.1'
8201428
1.2
8200255
1.4
8200271
1.5
8203507
N5
8210262
1.4
8210296
NS
8207169
1.0
8201337
1.1
8201394
3..
0
8203002
1.0
8205254
1.0
8205270
0.9
8200339
I.
0
8203481
1.0
8210387
1.2
8207177
0.7
8207235
1.1
8200511
1.6
8205155
1.1
­
Total
composite
(
9)
21.4
Date'
composited:
3/
1/
84
Vol
ati
1e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.
I
10
1.1
10
1.0
20
0.8
2
1.1
a.
NS
NS
1.4
4
NS
NS
0.9
7
0.9.
20
1.0
20
1.5
20
1.0
4
1.2
3
0.9
10
1.0
10
1.0
20
1.2
20
1.4
IS
1.2
0
1.4
10
­
2i.
I
c­
19
Census
Division
=
EN,
Age
Group
=
45
+
Years,
Composite
2
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
g>
.
Volatile
organic
composite
amount
added
(
g)
Approx
inate
mass
remaining
(
9)

8201220
1.7
1.8
5
8201261
1.7
1.6
5
8201279
1.8
1.5
10
8201444
1.5
1.7
5
8205106
1.3
1.3
4
8205239
1.0
1.5
1
8302853
1.7
1.4
5
8200115
1.4
1.2
4
8200156
.
l.
6
1.5
2
8207946
1.1
0.5
5
8205189
1.2
1.6
2
8205205
1.6
1.3
2
8200420
1.0
0
0
8200446
1.6
1.4
3
8210163
NS
NS
NS
8210213
1.6
1.6
2
8210395
1.7
1.6
2
820s13a
1.4
1.1
2
8203507
1.3­
0­
0
22.6
Total
composite
(
9)
26.2
Date
composited:
3/
1/
84
c­
20
000160
..
.
.;.
'

L
Census
Division
=
EN,
Age
Group
=
15­
44
Years,
Composite
3
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8201295
1.2
8206898
1.0
8205114
1.1
8205197
1.7
8205262
1.0
8302838
1.2
8200131
0.4
8200172
1.0
8210155
1.1
8210239
NS
8201196
0.9
8203004
1.2
8206831
1.3
8205296
0.9
8200198
1.2
8203473
1.0
8210130
G
8210361
NS
8207193
1.3
8207268
1.0
.
8210338
0.9
0.88207136
­
Total
composite
(
9)
20.2
Date
composited:
3/
1/
84
Volatile
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.5
10
1.6
15
0.9
10
1.1
6
0.8
6
1.1
6
0
0
0.8
0
1.1
10
NS
NS
0.8
6
1.0
4
1.5
10
1.0
6
0.8
1
1.
I
4
NS
NS
NS
NS
1.4­
10
1.1
20
1.2
15
0.8
20
­
19.6
c­
21
000261
Census
Division
=
EN,
Age
Group
=
45
+
Years,
Composite
3
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8201329
1.9
8205213
1.6
8205221
1.8
8200495
0.8
8210197
NS
.
8210304
NS
8210312
1.9
8207151
2.3
8207227
1.7
8201253
1:
6
8201303
1.6
8201402
I
1.4
8205122
1.4
a2o5247
1.6
8302820
NS
8200479
1.6
8207219
2.0
­
Total
composite
(
9)
23.2
Date
composited:
3/
1/
84
Vo
1ati1
e
Approx
i
mate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.5
8
1.3
2
1.5
8
0
0
NS
NS
NS
NS
1.7
2
2.0
5
1.9
5
1.6
5
1.6
5
1.8
2
1.5
0
2.2
0.5
NS
NS
1.3
2
1.5
­
8
21.4
c­
22
000162
Census
Division
=
WN,
Age
Group
=
0­
14
Years,
Composite
1
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
Vol
ati
1
e
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)
1,

8201980
1.0
1.5
1
8205478
2.0
2.4
2.5
8205551
1.4
1.1
0
8205577
1.1
0
0
8205619
2.0
0
0
8205635
2.0
2.4
5
8205668
2.5
1.8
5
8205569
2.5
3.5
3
8205684
'
1.3
2.7
1.0
8205692
1.5
0
0
8205734
2.0
1.5
1
8205783
2.3
1.1
0
8201949
1.8­
0.9­
0
18.9
Total
composite
(
9)
23.4
Date
compos
ited:
2/
28/
84
C­
23
000163
Census
Division
=
WN,
Age
Group
=
15­
44
Years,
Composite
1
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
'
401
ati?
e
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8202012
1.2
1.6
10
8210833
0.9
1.0
20
8205486
0.9
1.2
10
8205536
1.4
1.9
7
8205544
1.1
1.3
7
8205585
1.1
1.0
10
8205601
1.1
0.9
8
8205643
1.1
1.2
6
8205676
1.2
1.5
1
8205718
1.2
1.5
4
8205742
1.7
1.7
2
8210759
1.2
1.1
10
8205593
1.2
1.0
5
8205627
1.6
1.2
20
8205700
1.3
1.0
10
8205759
1.2
1.1
10
8205767
1.2
.
­
1.4­­
5
21.6
Total
coinposite
(
9)
20.6
Date
composi
ted:
2/
29/
84
C­
24
000164
Census
Division
=
WN,
Age
Group
=
45
+
Years,
Composite
1
FY
82
specimen
no.
Semivol
eti
1
e
organic
composite
amount
added
(
9)
Volatile
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8201964
1.7
1.5
10
8202004
1.6
I.
7
5
8210783
1.5
1.5
5
8210841
1.5
1.6
10
8205429
1.7
1.4
5
8205452
1.7
1.6
5
8205502
1.1
1.3
5
8205510
1.5
1.5
5
8201998
1.2
1.1
5
8210791
1.4
1.1
5
8205395
1.8
1.8
1
8205403
1.6
1.9
5
8205437
1.5
1.6
2
8205445
1.7
1.0
2
8205650
1.0­
1.0­
2
21.6
Total
composite
(
9)
22.5
Date
composited:
2/
28/
84
c­
25
000165
Census
Division
=
WN,
Age
Group
=
45
+
Years,
Composite
2
FY
82
specimen
no.
Semivolatile
organic
composite
..
amount
added
(
9)
Vol
ati
1e
organic
composite
amount
added
(
9)
ApproxiEate
mass
remaining
(
9)

8201956
1.4
1.2
5
8202038
1.4
1.3
15
8202053
1.6
1.5
15
8210817
1.3
1.3
5
8205411
1.3
1.1
5
8205494
1.2
1.2
9
8205809
1.3
1.1
0
8201972
1.4
1.4
8
8202020
1.4
1.1
6
8202046
1.5
1.2
10
8210767
1.3
1.3
5
8205460
1.6
1.1
8
8205528
1.4
1.2
10
8205775
1.3
1.3
15
8205726
2.0­
1.0­
2
18.3
Total
composite
(
9)
21.4
Date
composited:
2/
28/
84
C­
26
000166
Census
Division
=
SA,
Age
Group
=
0­
14
Years,
Composite
1
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8201113
1.0
8303042
1.4
8202145
1.2
8204059
1.3
8202277
0.9
8203572
1.2
8203978
0.9
8202327
1.4
8202343
1.
I
8202426
0.9
8200149
1.1
8200222
0.6
8203986
1.3
8202350
0.8
a201089
1.3
8202129
0.8
8202160
0.9
8202194
0.
a
a203952
0.8
8202244
1.0
Total
composite
(
9)
20.7
Date
cornposited:
2/
29/
84
Vofati
le
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.0
10
1.6
.
o.
5
0
0
0
0
0.9
4
1.4
0.5
0
0
0.8
10
1.5
1
1.7
4
0.7
0
0
0
0.3
0
0.8
15
1.0
2.5
0
0
0
0
0
­
0
0
0
­
15
0.9
12.6
C­
27
000167
Census
Division
=
SA,
Age
Group
=
15­
44
Years,
Composite
1
Semivol
ati
1
e
Vol
ati
1e
FY
82
organic
composite
organic
composite
specimen
no.
amount
added
(
9)
amount
added
(
9)

8203515
1.0
8203671
1.3
8203762
1.1
8203796
1.1
8203853
1.0
8202269
1.1
8202509
0.9
8207003
0.8
8201105
0.9
8203895
1.1
8203929
1.5
8204000
0.9
8202251
1.0
8202616
0.8
8207086
0.9
8203606
0.8
8201139
1.0
8201147
0.8
8203788
1.0
8203820
0.9
8208316
0.9
8110041
NS
8200206
1.3
8200248
0.8
8204042
1.0
8202434
1.1
8202525
1.4
­

Total
composite
(
9)
26.4
Date
composited:
2/
29/
84
1.0
0
0
0.9
0.9
1.1
1.0
\,

0.9
0.8
1.0
 
1.1
0.7
0.7
0.8
1.5
0.8
0.8
1.3
0.9
0.9
0.8
NS
0.6
0.7
1.4
1.2
1.0
­
22.8
C­
28
Approximate
mass
remaining
(
9)

10
0
0
2
1
10
2
1
10
5
0
0.5
2
5
0
3
4
2
2
1
1
NS
0
0
0
10
4
000168
Census
Division
=
SA,
Age
Group
=
45
+
Years,
Composite
I
FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
Val
ati1e
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8206963
0.8
0.7
4
8203556
0.8
0.7
10
8203580
0.7
0.6
'
6
8201014
0.7
0.6
6
8200073
0.6
0.6
a
8202186
.
0.5
0
0
8203747
0.6
0.8
.
o
8203879
0.5
0.6
0
8204034
0.6
0.7
7
8202384
0.7
0.7
20
8206989
0.9
1.2
10
8207037
0.6
0.7
6
3203598
1.4
0.9
15
82.01055
0.9
0.8
.
6
8303083
NS
NS
NS
8203705
0.7
0.8
7
8203713
0.6
0.9
3
8208332
0.7
0.7
a
8202301
0.9
0.7
'
a
8207011
0.8
0.7
S
8iioosa
NS
NS
NS
8200164
I.
2
0
0
8203655
1.0
0
0
8203721
0.8
0
0
8202210
1.0
0.6
1s
8202392
1.0
0.6
20
8202558
1.0
0.8
10
8202632
NS­
NS­
NS
15.4
Total
composite
(
9)
20.0
Date
composited:
2/
29/
84
C­
29
0003.69
Census
Division
=
SA,
Age
Group
=
0­
14
Years,
Composite
2
FY
82
specimen
no,
Semivolatile
organic
composite
amount
added
(
9)
Vo
'
Iati
1
e
organic
composite
amount
added
(
9)
Approxi
mate
mass
remaining
(
9)

8303257
1.8
1.6
2
8208506
0.3
0
0
8202533
,8202368
1.6
1.2
2.1
2.3
5
1
8303273
1.2
1.2
1
8200305
1.0
0
0
8202079
8201121
1.2
2.3
0.6
1.9
0i
8303232
1.8
1.5
0
8204018
0.6
0
0
8202285
1.7
1.7
5
8202376
1.6
1.5
8
8303067
1.1
,
0.8
0
8303091
1.7­
I.
5­
0
16.7
­

Total
composite
(
9)
19.1
Date
composited:
3/
1/
84
C­
30
Census
Division
=
SA,
Age.
Group
=
15­
44
Years,
Composite
2
.
k.

FY
82
specimen
no.

8207078
8302986
8203887
8208472
8110025
8201154
8202111
8203770
8207060
8207144
8203622
8200321
8203754
8202103
8203739
8202236
8202608
8202335
8202442
8208522
8202459
8203994
8202400
8203804
8203911
Semivolatile
.
organic
composite
amount
added
(
9)

0.7
NS
0.8
1.0
NS
0.7
0.9
0.6
0.9
0.7
1.3
0.7
1.1
0.9
0.9
1.0
1.0
0.7
0.8
NS
1.0
1.0
1.1
1.0
0.7
­
Total
composite
(
9)
19.5
Date
composited:
3/
1/
84
I
C­
31
..
.
.

Vo
1ati
?
e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

0.8
1
NS
NS
0.9
0.5
0.7
0.5
NS
NS
0.8
10
0.7
10
0.7
2
0.7
1
0.8
6
0.8
10
0.6
2
1.2
5
1.1
1
1.4
0
1.1
20
1.2
10
0.8
15
0.6
5
NS
NS
0.6
20'
0.6
0
0.8
15
0.9
1
0.9
­
4
18.7
000171
Census
Division
=
SA,
Age
Group
=
45
+
Years,
Composite
2
Semivolatile
Volatile
Approximate
FY
82
organic
composite
organic
composite
mass
specimen
'
no.
amount
added
(
9)
amount
added
(
9)
remaining
(
9)

____
___~

8206971
8110033
8202061
8207052
8203531
8201006
8203812
8203861
8208514
8202483
8202574
8202178
8204026
8208480
8202202
8202467
8202590
8201022
8202137
8202152
8208399
8202418
8202624
Total
composite
(
9)
1.2
1.1
2
NS
NS
NS
0.8
0.7
0
1.6
1.2
2
1.1
1.3
5
1.3
1.3
5
1.0
0.9
0
1.1
1.1
2
NS
NS
NS
1.6
1.4
5
1.4
1.1
10
1.1
1.4
1
1.1
0.9
1
1.2
1.2
5
1.3
1.0
0
1.1
0.9
8
1.2
1.3
5
1.6
1.3
10
1.1
0.4
0
1.3
1.0
1
1.3
1.2
2
3..
3
1.3
10
1.4
1.2
­­
5
26.1
23.2
Date
composited:
3/
1/
84
C­
32
OOOiY2
Census
Division
=
SA,
Age
Group
=
15­
44
Years,
Composite
3
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8203523
0.8
8203546
0.7
8201071
0.9
'

8202087
1.1
8203697
0.4
8208407
1.5
8109993
NS
8302937
0.9
8303240
1.3
8200362
1.1
8203937
1.2
8208365
0.6
8207110
0.7
8110066
NS
8303117
0.7
,

8202293
0.8
8202582
0.6
,

8303109
1.5
8200347
0.7
8203960
1.0
8202491
NS
8202517
1.4
­
Total
composite
(
9)
17.9
Date
cornposited:
3/
1/
84
Volatile
Approximate
organic
cornposite
mass
amount
added
(
9)
remai
ning
(
9)

0.6
8
1.2
3
0.7
4
0.7
1
0
0
0
0
NS
NS
0.8
8
0.6
5
0
0
0
0
0.7
0
0.9
6
NS
NS
0.7
5
0.9
6
0.6
10
0.9
5
0
0
0
0'
NS
MS
0.8
­
10
10.1
c­
33
000173
Census
Division
=
SA,
Age
Group
=
45
+
Years,
Composite
3
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8207029
1.7
8302960
2.7
8201048
2.0
8201063
2.0
8110009
NS
8200123
1.8
8202566
2.4
8201030
2.2
'
8303125
2.0
8203846
i.
2
­
Total
composite
(
9)
18.0
Date
cornposited:
3/
1/
84
..
Vo
1
ati
1e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

0
0
2.2
2
2.3
0
2.5
2
NS
NS
0.6
0
2.5
5
1.9
6
1.8
2
0
­
0
13.8
c­
34
oooi74
Census
Oivision
=
SA,
Age
Group
Semivol
ati
1e
FY
82
organic
compos
ite
specimen
no.
amount
added
(
9)

8203838
1.3
8208415
NS
8202228
1.4
8207128
1.4
8203663
1.4
8202541
1.6
!
8207102
1.4
8302978
1.7
8203689
1.4
8202319
1.5
8303059
1.3
8208530
NS
8202475
*
2.0
1.8
8202491
­
Total
composite
(
9)
18.2
Date
cornposited:
3/
1/
84
c­
35
=
15­
44
Years,
Composite
4
Vol
ati
1e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

0.6
0
NS
NS
1.4
10
1.3
1
1.4
2
1.5
20
1.2
0
1.7
25
1.6
0.5
1.9
20
1.8
4
NS
NS
1.9
15
1.5
­
20
17.8
000175
Census
Division
=
SA,
Age
Group
=
45
+
Years,
Composite
4
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)
Volatile
organic
composite
amount
added
(
9)
Ap
p
roximate
mass
remaining
(
9)

8206955
5.3
4.5
0
8206948
.
3.3
0
0
8207045
3.0
­
2.6
0
8206997
4.9
4.5
0
1.18203945
­
0­
0
Total
composite
(
9)
17.6
11.6
Date
composited:
3/
1/
84
C­
36
Census
Division
=
ES,
Age
Group
=
0­
14Years,
Composite
1
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8200628
0.8
8200636
0.6
8200685
2.2
8200792
0.
a
8200800
1.0
8200867
0.8
82018ai
0.8
8201915
0.6
8204190
0.7
8204208
1.0
8204216
1.4
8204273
0.9
8204497
1.1
8200677
0.5
8200768
0.8
8200883
1.2
8201923
1.0
8201931
1.6
8204174
1.5
8204182
1.5
8204224
1.1
8204240
1.0
8204257
1.3
8204406
1.2
8200560
1.1
8204299
1.6
Total
composite
(
9)
28.1
Date
composi
ted:
2/
29/
84
Volatile
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

0
0
0.8
2
0.6
2
0.6
1
0.9
5
0.8
2
1.9
2
0.6
2
1.0
2
1.2
1
1.0
1
1.0
1
1.0
2
0.6
2
1.8
2
1.1
2
1.2
3.
1.2
0
1.
I
2
1.4
1
1.1
2
0.8
2
1.3
2
0.7
2
0.8
2
1.1
2
­
25.6
c­
37
000177
Census
FY
82
specimen
no.

8200586
8200727
8201865
8204232
8204281
8204430
8204554
8200610
8200719
8200818
8201873
8204265
8204307
8204323
8200750
8204489
Division
=
ES,
Age
Group
SeRi
vol
ati
1
e
organic
composite
amount
added
(
9)

1.2
1.3
1.3
1.0
1.3
1.0
1.3
1.
I
1.7
1.1
1.3
1.0
1.3
1.4
1.5
1.1
­
=
15­
44
Years,
Composite
1
Vol
ati
1
e
organic
composite
amount
added
(
9)

1.1
1.2
1.3
1.4
1.1
1.1
1.5
1.0
0.3
1.2
1.2
1.1
1.2
1.4
1.4
1.5
­
19.0
Approximate
mass
remaini
ng
(
9)

20
6
6
2
4
3
3
4
4
10
10
3
2
4
5
5
Total
composite
(
9)
19.9
>

Date
composi
ted:
2/
29/$
4
C­
38
Census
Division
=
ES,
Age
Group
=
45
+
Years,
Composite
1
Semivolatile
FY
82
organic
composite
specimen
no.
amount
added
(
9)

8200644
1.1
8200669
1.2
8200735
1.1
azo4398
1.2
a204414
1.4
8204443
1.3
8204455
1.4
8204463
1.2
8204513
1.2
8200552
1.2
8200776
1.1
8200784
1.4
8200834
1.4
8200875
1.0
8204422
1.2
8204521
1.2
8204547
1.1
Total
composite
(
9)
20.7
Date
composited:
2/
29/
84
Vo
1
ati1
e
Approximate
organic
composite
mass
amount
added
(
9)
remaining
(
9)

1.3
5
1.2
4
1.0
2
1.4
2
1.4
2
1.3
2
1.0
2
1.2
2
1.2
2
1.1
2
1.0
3
1.6
4
1.2
5
1.0
2
1.2
2
1.2
2
­
3
1.3
20.6
c­
39
000179
Census
Division
=
ES,
Age
Group
=
15­
44
Years,
Composite
2
~

FY
82
specimen
no.
Semivolati
le
organic
composite
amount
added
(
9)
Volatile
organic
compos
i
te
amount
added
(
9)
Approximate
mass
remaining
(
9)

8200578
1.5
1.5
5
8200594
1.2
0.7
0
8200529
1.9
2.0
10
8200693
0.9
2.0
0
8200826
1.7
1.6
4
8204315
1.7
1.6
2
­
8204331
1.7
1.6
2
8204356
1.5
1.3
2
8204539
2.2
1.6
1
8204372
1.9
2.0
2
8200743
8200859
1.8
i.
4
1.1
1.4
5
5
8200891
0.5
0.1
5
82oia99
1.5
1.4
5
8204349
1.5
1.7
2
8204364
8204380
1.2­
1.6
1.2
1.5­
2
2
24.3
Total
composite
(
9)
25.7
Date
composited:
3/
1/
84
.
.,­

C­
4
0
000180
Census
Division
=
ES,
Age
Group
=
45
+
Years,
Composite
2
FY
82
specimen
no.
Semivolati
1e
organic
composite
amount
added
(
9)
Vol
;
ti
1e
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8200537
2.2
2.3
'.
4
8200602
1.9
1.8
.
I
8200651
2.1
1.9
4
8200701
2.6
2.4
5
8200842
2.4
3.4
6
8200545
2.1
*
.
'
2.0
4
8204471
2.5
1.8
.
2'
8204505
2.9
1.6
1.
8204562
2.4
2.1
­­
2
Total
composite
(
9)
21.
I
19.3
Date
composited:
3/
1/
84.

C­
41
Census
Division
=
WS,
,
Age
Group
=
0­
14
Years,
Composite
1
,,

FY
82
specimen
no.
Semivolatile
organic
composite
amount
added
(
9)
Volatile
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8202848
1.2
1.2
2
8206773
1.1
1.1
0
8206781
0.3
0
0
8206799
0.6
0
0
8202798
1.8
1.6
3
8202897
1.2
.
1.4
3
8206757
1.2
0.7
0.
8206807
0.3
0
0
8206849
0.5
0
0
8202889
NS
NS
NS
8206732
0.4
0
0
8206755
a.
7
0
0
8206823
.
1.3
0
0
8206815
:­,
0.5­
0­
0
6.0
Total
composite
(
9)
11.1
Date
composi
ted:
2/
29/
84
C­
42
000182
Census
Division
=
WS,
Age
Group
=
15­
44
Years,
Composite
2
FY
82
specimen
no.
Semivolatile
.
organic
composite
amount
added
(
9)
Volati
7e
organic
composite
amount
added
(
9)
Approxi
mate
mass
remaining
(
9)

8202640
1.7
1.3
25
8202723
0.9
0.8
3
8202772
1.0
0.8
1
8202988
1.5
1.1
8
8206625
0.9
1.4
25
8206690
0.8
1.7
8
8206708
1.8
1.2
15
8202665
.
1.2
0.9
25
8202756~
1.7
1.0
0
8202780
a
a
a
8202806 
1.3
1.2
1
8202939
1.1
1.7
.4
8206583
1.5
1.4
25
8206617
1.0
1.6
20
8206633
1.2
1.0
15
8206658
1.1
1.0
15
8202863
0.9
1.
I
15
8202970
1.0
1.0
5
820292I
1.1
1.3
5
8202889
1.0­
0.9­
20
22.4
Total
composite
(
9)
22.7
Date
composited:
2/
29/
84
aSample
included
in
the
45
+
composite.

c­
43
000183
Census
Division
=
WS,
Age
Group
=
45
+
Years,
Composite
1
FY
82
specimen
no.
Semivolati
1
e
organic
composite
amount
added
(
9)
Volatile
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8202681
0.8
0.8
4
8202699
0.9
0.9
9
8202749
1.1
1.0
8
820282.4
0.8
0.8
3
8202830
0.9
1.0
5
8206450
0.9
1.1
5
8206500
0.9
1.0
5
8206526
1.0
0.8
5
8206724
1.1
0.9 
10
8202657
1.2
1.0
8
8202673
i
0.9
1.0
8
8202707
.
0.9
LO
5
8202715
0.9
0.8
8
8202731
1.1
0.9
5
8202855
0.9
0.9
4
8206484
1.3
1.4
8
8206534
I
1.0
0.9
9
8206542
1.1
1.0
.
10
8206567
0.9
0.8
10
8206716
0.9
1.0
8
8206641
0.9
1.0
9
8206609
1.0
1.0
8
8202780
1.0­
1.0­
8
22.0
%?

Total
composite
(
9)
22.4
Da.
te
composited:
2/
29/
84
c­
44
.

Census
Division
=
WS,
Age
Group
=
15­
44
Years,
Composite
2
FY
a2
specimen
no.
Semivol
ati
1e
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8202764
1.2
5
8202962
1.0
10
8206476
1.2.
10
8206492
0.7
10
8206575
.
1.1
10
8206666
1.2
10
8206740
1.1
10
8202822
1.3
1
8202871
1.1
5
8202913
'
1.4
5
8202947
1.6
10
8206559
0.9
10
8206591
1.3
5
8206674
1.1
10
8206682
1.5
10
8202954
1.9
5
8202996
0.9
10
8206518
1.4­
5
Total
composite
(
g>
21.9
Date
composited:
3/
1/
84
Vol
at­
i
le
organic
composite
amount
added
(
9)

1.8
1.3
0.9
1.0
1.1
1..
0
0.8
1.7
1.6.
1.5
1.3
0.9
1.1
1.2
1.4
1.3
1.0
1.0
­
21,9
c­
45
000185
Census
Division
=
MO,
Age
Group
=
0­
14
Years,
Composite
1
Semivolatile
Volatile
Approximate
FY
82
organic
composite
organic
composite
mass
specimen
no.
amount
added
(
g}
amount
added
(
9)
remaining
(
9)

8110199
0.8
8110207
2.6
8110256
1.0
8110272
0.2
8110116
2.4
8206468
1.3
8110157
0.7
­
Total
composite
(
9)
9
­
0
Date
composited:
2/
29/
84
0
2.4
0
0
2.7
0
0
­
5.1
C­
46
000186
Census
Division
=
MO,
Age
Group
=
15­
44
Years,
Composite
1
FY
82
specimen
no.
Semivolati
le
organic
composite
amount
added
(
g)
Volatile
organic
composite
amount
added
(
9)
Approximate
mass
remaining
(
9)

8110090
1.4
1.4
6
8110124
1.3
,
1.2
1
8110215
1.3
2.1
15
8110231
1.4
1.4
10
8110306
NS
NS
NS
8110397
NS
NS
NS
a204067
1.5
1.5
'
7
8204083
1.7
1.2
10
8204158
1.,
8
1.5
IS
8110108
1.3
1.3
10
8110132
2.0
1.5
2.0
8110165
1.4
1.4
5
8110249
1.8
2.8
0
8110348
NS
NS
NS
8110363
NS
NS
NS
8110371
NS
NS
NS
8110488
NS
NS
*
NS
­
1.5
8204075
1.4
­
10
Total
composite
(
9).
18.3
.
18.8
Date
composited:
2/
29/
84
c­
47
000187
Division
=
MO,
Age
Group
=
45
+
Years,
Composite
1
Census
FY
82
specimen
no.

8110140
8110173
8110181
8110330
8110421
'
8110439
8110454
8110462
8204117
8204133
8204141
8204166
8110264
8110280
8110298
8110322
8110389
8110447
8110470
8204109
8204125
Sernivol
ati
1e
organic
composite
amount
added
(
9)
Vol
ati1
e
organic
composite
amount
added
(
9)

2.2
2.7
2.0
NS
NS
NS
NS
NS
2.1
.

2.0
2.1
2.0
2.6
NS
NS
NS
NS
NS
NS
2.2
2.5
­
22.4
Approximate
mass
remaining
(
9)

5
0.5
4
NS
NS
NS
NS
NS
5
5
5
4
5
NS
NS
NS
NS
NS
NS
5
5
2.0
2.0
2.2
NS
NS
NS
NS
NS
2.0
2.1
'

2.1
2.2
2.
I
NS
NS
NS
NS
NS
NS
2.2
2.
I
­
21.0
Total
composite
(
9)

Date
composited:
2/
29/
84
C­
48
000188