Document ID: EPA-HQ-OPPT-2002-0066-0022
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2002-12-05T05:00Z

I
OPP7­
2002­
0066­
0021
United
States
Office
of
EPA­
560/
5­
86­
035
Environmental
Protection
Toxic
Substances
December,
1986
Agency
Washington
DC
20460
­.­_­
PB87177218
Toxic
Substances
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REPRODUCEDBY
US.
DEPAKrMENTOFCOMMERCE
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TECHNICAL
INFORMATKINSERVICE
SPRINGFIELD,
VA
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1
f.
TITLE
ANO
s~
3rlTLC
Broad
Scan
Analysis
of
Human
Adipose
Tissue
Volume
1
­
Executive
Summary
7.
At;
TMOr7(
fl
John
S.
Stanley
Midwest
Research
Institute
425
Vol
ker
Boul
ward
Kansas
City,
Missouri
64110
F~
eldStudies
Branch
(
TS­
798)
Oesian
Development
granch/
ExDosure
Evaluation
Division
J.
Remners
and
2.
Robinson,
blork
Assignment
Managers
J.
Breen
and
C.
Stroun.
Pra
ar­
m
16.
aasTaAcT
'
5.
REPOAT
DATE
December
1986
6.
PERFORMING
0RGANlZAT;
ON
C3OE
Midwest
Research
Institute
8.
PERFCRMING
ORGANIZATION
REPOST
'
40
8821­
A(
01
)

11.
CONiRACT/
GaXNr
NO.

68­
02­
3938
i
68­
02­
4252
I
The
National
Human
Adipose
Tissue
Survey
(
NHATS)
provides
the
U.
S.
EPA
with
a
unique
capabi
1
ity
for
monitoring
human
eiposure
to
potential
ly
toxic
substances
that
per
sist
in
the
environment.
NHATS
is
an
annual
program
to
collect
and
chemically
analyze
adipose
tissues
from
a
cross­
section
of
the
general
U.
S.
population.
Historically,
the
analysis
of
the
tissues
has
focused
on
PCBs
and
organochlorine
pesticides.
EPA's
Office
of
Toxic
Substances
(
OTS)
has
developed
an
aggressive
approach
to
provide
a
cornprehensive
assessment
of
potentially
toxic
substances
in
human
adipose
tissue.
A
broad
scan
analysis
concept
was
introduced
beginning
with
specimens
collected
in
fiscal
year
1982.
The
tissues
were
analyzed
as
composites
based
on
the
nine
U.
S.
Census
divisions
and
three
age
groups.
The
composites
were
analyzed
for
volatile
and
semivolatile
organics
at
the
parts
oer
billion
level
and
PCDD
and
PCDF
at
the
parts
per
trillion
level.
Several
tissue
samples
were
analyzed
by
individually
coupled
plasma­
afornic
emission
spectroscopy
(
ICP­
AES)
and
neutron
activation
analyses
(
NAA).
This
report
proviaes
a
synopsis
of
each
of
these
analytical
efforts.

7.
<
EY
'
WORDS
AN0
OOCUMENT
ANALYSIS
5
CSCR
t
Pf3
AS
Ib.
lOENTIFIERS/
OPSN
ENOE.
3
'
LAMS
IC'.
C3SA.
T;
fk:
d!
CfOUD
tuman
Adi
oose
Tissue
I
I
I
lo1ati
1
e
Organic
Compounds
Analysi
s
iemivol
aci
1e
Organic
Compounds
'
olychlorinated
Oibenzo­
o­
ai
oxi
ns
(
PCDD)
'
0
1
yc
hl
or?
nated
Di
benzocrans
(
PCDF)
'
CB
BROAD
SCAN
ANALYSIS
OF
HUMAN
ADIPOSE
TI.
SSUE:
VOLUME
1:
EXECUTIVE
SUMMARY
by
John
S.
Stanley
FINAL
REPORT
EPA
Contract
No.
68­
02­
4252
Work
Assignment
.
No.
21
MRI
Project
No.
8821­
A01
December
31,
1986
,

Prepared
For:

I
National
Human
Monitoring
Program
Field
Studies
Branch
(
TS­
798)
Design
and
Development
Branch
I
Office
of
Toxic
Substances
U.
S.
Environmental
Protection
Agency
401
M
Street.
S.
W.
Was
hi
ngton,
DC
20460II
Attn:
Ms.
Janet
Remmers
and
Mr.
Philip
Robinson,
Work
Assignment
Managers
Dr.
Joseph
J.
Breen
and
Ms.
Cindy
Stroup,
Program
ManagersE
i
..
hi
E
DISCLAIMER
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
S
products
does
not
constitute
Agency
endorsement
or
recommendation
for
use.

i
PREFACE
This
executive
summary
is
the
first
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.
I.

This
first
volume
summarizes
data
generated
from
all
analysis
efforts.
Volumes
I1
thro­
ugh
V
deal
specifically
with
the
chemical
analysis
of
the
NHATS
'
composites.
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
35.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
I:
Executive
summary.
EPA
560/
5­
86­
035.

­
Stanley
JS.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
11:
Volatile
organic
compounds.
 PA
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
JS.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
IV:
Polychlorinated
dibenzo­
p­
dioxins
(
PCDDs)
and
polychlorinated
dibenzofurans
(
PCDFs)
EPA
560/
5­
86­
038,

*
Stanley
35,
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
3938
and
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.
Kathy
Boggess,
Mr.
John
Onstot,
and
Dr.
Thomas
Sack.
The
compositing
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).

Program
Manager
J$
n
E.
Going
iii
f.
,
63sit.
635
01rector
.,
iU
Chemical
Sciences
Department
I
I
I.

11.

111.

IV.

Appendix
A
TABLE
OF
CONTENTS
Introduction.
.......................

A.
Broad
Scan
Analysis
Strategy
............
8.
Work
Assignment
Objectives
............

Project
Summary
......................

A.
B.
C.
D.
E.
Collection
and
Storage
of
NHATS
Specimens.
....
Volatile
Organic
Compounds
............
Semivolatile
Organic
Compounds
..........
PCDDandPCDF.
..................
Trace
Elements
..................
Page
1
1
1
2
2
3
4
16
24
27
27
27
28
29
30
31
Recommendations
......................

A.
Volatile
Organic
Compounds
............
B.
Semivolatile
Organic
Compounds
..........
C.
PCDDandPCDF.
..................
D.
Trace
Elements
..................

References.
........................

­
Glossary
of
Terms.
...................

V
I
LIST
OF
TABLES
Tab1e
1
Incidence
of
Detection
of
Target
Volatile
Organic
Compounds
in
the
NHATS
FY82
Composite
Specimens.
....

2
Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
Northeast
Census
Region.
................

3
Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human.
Adipose
Tissue
from
the
Page
5
6
t
8
9
11
12
14
15
17
18
z
19
4
5
8
9
10
11
12
13
South
Census
Region.
..................

Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
North
Central
Census
Region.
..............

Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
West
Census
Region
...................

Incidence
of
Detection
of
Target
Semivolatile
Organic
Compounds
in
the
NHATS
FY82
Composite
Specimens.
....

Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
West
Census
Region
.................

Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
Northeast
Census
Region.
..............

Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
North
Central
Census
Region.
............

Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
South
Census
Region.
.................

Lipid­
Adjusted
Concentration
of
PCDD
and
PCDF
in
the
NHATS
FY82
Composite
Specimens
...........

PCDD
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specl mens
from
the
Northeast
Census
Region
.......

PCDD
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specimens
from
the
West
Census
Region.
..........

J
vi
LIST
OF
TABLES
(
concluded)

Tab1e
Page
14
PCDD
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specimens
from
the
South
Census
Region
.
.
.
.
.
.
.
.
.
20
15
PCDO
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specimens
from
the
North
Central
Census
Region
.
.
.
.
.
21
16
Concentration
(
pg/
g)
for
Trace
Elements
in
Adipose
Tissue
Determined
by
ICP­
AES
Analysis.
.
.
.
.
.
.
.
.
.
25
17
Summary
of
Data
for
Trace
Elements
(
pg/
g)
Identified
in
Nine
Human
Adipose
Tissue
Specimens
by
NAA
.
.
.
.
.
.
.
26
vi
i
­­
c
LIST
OF
FIGURES
Figure
Page
1
Flow
scheme
for
analysis
of
semivolatile
organic
compounds
in
human
adipose
tissue.
...........
10
2
PCDD
and
PCDF
distribution
in
the
general
U.
S.
population
by
age
group.
................
22
3
Comparison
of
PCDD
and
PCDF
concentration
(
based
on
wet
tissue
weight)
profiles
for
Sweden,
the
general
U.
S.
population,
and
upstate
New
York.
.........
23
F
viii
I.
INTRODUCTION
The
U.
S.
Environmental
Protection
Agency's
Office
of
Toxic
Substances
(
EPA/
OTS)
maintains
through
the
National
Human
Adipose
Tissue
Survey
(
NHATS)
a
unique
program
for
estimating
the
general
population
exposure
to
toxic
organic
chemicals.
NHATS
is
the
main
operative
program
of
the
National
Human
Monitoring
Program
(
NHMP).
The
NHMP
was
first
established
by
the
U.
S.
Public
Health
Service
in
1967,
and
was
subsequently
transferred
to
EPA
in
1970.
During
1979
the
program
was
transferred
within
EPA
to
the
Exposure
Evaluation
Division
of
OTS.

NHATS
is
an
annual
program
to
collect
and
chemically
analyze
a
nationwide
sample
of
adipose
tissue
specimens
for
the
presence
of
toxic
compounds.
The
objective
of
the
program
is
to
detect
and
quantify
the
prevalences
of
toxic
compounds
in
the
general
population.
The
specimens
are
collected
from
autopsied
cadavers
and
surgical
patients
according
to
a
statistical
survey
design
(
Lucas
1981).
The
design
ensures
that
specified
geographic
regions
and
demographic
categories
are
appropriately
represented
to
permit
valid
and
precise
estimates
of
baseline
levels,
time
trends,
and
comparisons
across
subpopulations.

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
Historically,
organochlorine
compounds
and
polychlorinated
biphenyls
(
PCBs)
have
been
selected
for
evaluation.

A.
Broad
Scan
Analysis
Strategy
EPA/
OTS
has
developed
an
aggressive
strategy
to
expand
the
use
of
the
NHATS
program
so
as
to
provide
a
more
comprehensive
assessment
of
TSCArelated
substances
that
persist
in
the
adipose
tissue
of
the
general
U.
S.
population.
The
NHATS
specimens
collected
during
fiscal
year
1982
(
FY82)
were
selected
for
a
broad
scan
analysis
of
volatile
and
semivolatile
organic
TSCArelated
chemicals
and
trace
elements
(
Mack
and
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.
Data
reported
on
NHATS
specimens
up
to
the
FY82
collection
are
limited
to
organochlorine
pesticides
and
PCBs
based
on
packed
column
gas
chromatography/
electron
capture
detector
(
PGC/
ECD)
analysis.

B.
Work
Assignment
Objectives
The
objectives
of
this
work
assignment
were
(
1)
to
identify
appropriate
analytical
methods
for
a
broad
scan
analysis
of
human
adipose
tissue
based
on
high
resolution
gas
chromatography/
mass
spectrometry
(
HRGC/
MS)
detection
for
general
semivolatile
and
volatile
organic
compounds
and
multielemental
techniques
[
neutron
activation
analysjs
(
NAA)
and
inductively
coupled
emission
spectrometry
(
ICP­
AES))
for
toxic
trace
elements;
(
2)
to
conduct
preliminary
evaluation
of
the
analytical
procedures;
(
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
for
analytes
by
the
HRGC/
MS
as
specified
in
the
current
NHATS
strategy
(
Mack
and
Stanley
1984)
was
0.05
1
to
0.10
pg/
g);
and
(
4)
to
compare
the
data
generated
by
the
two
multielemental
techniques
through
the
analysis
of
nine
individual
NHATS
specimens.

The
broad
scan
analysis
approach
is
necessary
to
identify
additional
compounds
or
toxic
trace
elements
that
may
be
of
concern
to
EPA
under
the
mandates
of
TSCA.
The
multielemental
analysis
techniques
were
included
as
screening
procedures
to
provide
information
on
toxic
trace
elements
that
persist
in
human
adipose
tissue.

A
s'ummary
of
the
results
that
were
generated
from
the
FY82
NHATS
project
is
given
in
Section
11.
Recommendations
for
additional
methods
development
are
presented
in
Section
111.
Appendix
A
provides
a
glossary
of
the
terms
used
throughout
this
text.

11.
PROJECT
SUMMARY
The
broad
scan
analysis
task
has
resulted
in
the
development
and
preliminary
evaluation
of
HRGC/
MS
methods
for
the
measurement
of
volatile
and
semivolatile
organic
compounds
at
concentrations
ranging
from
0.001
to
2
pg/
g
in
human
adipose
tissues.
Procedures
based
on
selected
ion
monitoring
(
SIM)
techniques
have
provided
qualitative
analysis
for
complex
analytes
such
as
toxaphene.
The
sensitivity
of
the
SIM
technique
has
also
been
applied
to
the
determination
of
parts
per
trillion
(
picogram/
gram)
quantities
of
specific
polychlorinated
dibenzo­
2­
dioxin
(
PCDD)
and
dibenzofuran
(
PCDF)
congeners.
Two
multielement
analysis
techniques
were
evaluated
to
determine
the
levels
of
toxic
trace
elements
in
adipose
tissue.

The
results
of
this
broad
scan
analysis
activity
have
been
presented
in
part
at
the
American
Chemical
Society
Symposium
on
"
Exposure
Measurement
and
Evaluation
of
Methods
for
Epidemiology
Studies,"
Chicago,
IL,
September
1985;
the
Fifth
International
Dioxin
Symposium
in
Bayreuth,
FRG,
September
1985
(
Stanley
et
al.
1986);
13th
Annual
Federation
of
Analytical
Chemistry
and
Spectroscopy
Society
Symposium
on
"
Application
of
Mass
Spectrometry
in
Trace
Analysis,"
St.
Louis,
MO,
in
October
1986.

In
addition
to
these
reports
and
presentations,
a
detailed
method
protocol
for
the
determination
of
specific
semivolatile
organic
compounds
in
human
adipose.
tissue
was
prepared
and
submitted
for
peer
review
(
Stanley
1985).
This
analytical
method
is
undergoing
additional
validation
for
implementation
into
the
NHATS
program
for
routine
analysis.

The
results
of
the
method
development
and
sample
analysis
activities
are
reported
in
four
separate
reports
dealing
specifically
with
volatile
(
Stanley
1986a),
and
semivolatile
organics
(
Stanley
1986b),
PCDDs
and
PCDFs
(
Stanley
1986~)~
and
trace
elements
(
Stanley
and
Stockton
1986).
A
synopsis
of
the
results
based
on
each
analysis
effort
is
presented.

A.
Collection
and
Storage
of
NHATS
Specimens
The
adipose
tissue
specimens
were
originally
collected
during
FY82
(
October
1,
1981,
through
September
30,
1982)
for
determination
of
organo2
chlorine
pesticide
and
PCB
residues.
The
specimens
were
collected
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
(
airborne
levels)
of
solvents
or
metals.

The
adipose
tissue
specimens
were
sealed
in
glass
jars
and
frozen
(­
20
°
C)
following
collection.
The
specimens
were
shipped
in
insulated
coolers
packed
in
dry
ice.
The
FY82
specimens
were
originally
received
and
stored
at
EPA's
Toxicant
Analysis
Center
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.
The
procedures
for
preparation
of
the
composite
specimens
are
presented
in
detail
in
the
report
that
focuses
on
the
volatile
organic
analyses
(
Stanley
1986a).

8.
Volatile
Organic
Compounds
An
analytical
method
based
on
a
heated
dynamic
headspace
purge
and
trap
technique
was
developed
to
sample
volatile
organic
compounds
from
human
adipose
tissue.
The
volatile
organic
compounds
were
separated
and
detected
using
HRGC/
MS.
HRGC
was
selected
to
achieve
the
best
possible
separation
of
volatile
components.
MS
was
selected
as
a
detector
to
provide
the
necessary
specificity
to
positively
detect
the
volatile
compounds
present
in
adipose
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
that
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
desigh
prepared
by
the
EPA/
OTS
Design
and
Development
Branch
contractor,
Battelle
Columbus
Laboratories.
The
composite
samples
represent
the
nine
U.
S.
census
divisions
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
aldehydes,
ketones,
hydrocarbons,
and
carboxylic
acid
esters.
Additional
compounds
that
are
classified
as
aromatic,
halogenated
aliphatic,
and
halogenated
aromatic
compounds
were
detected
as
minor
constituents.

Quantitative
data
were
determined
for
17
specific
compounds.
The
predominant
target
analytes
that
were
noted
in
this
study
included
chloroform,
l,
l,
l­
trichloroethane,
benzene,
tetrachloroethene,
toluene,
chlorobenzene,
ethylbenzene,
styrene,
1,1,2,2­
tetrachloroethane,
1,4­
dichlorobenzene,
1,2dichlorobenzene
xylenes,
and
ethylphenol.

3
Several
compounds,
including
styrene,
the
xylene
isomers,
1,4­
dichlorobenzene
and
ethylphenol,
were
detected
in
all
composite
samples.
Table
1
presents
the
incidence
of
detection
for
the
selected
target
analytes
and
the
range
of
concentrations
observed.
Qualitative
summaries
of
the
incidence
of
detection
based
on
age
group
and
census
division
are
presented
in
Tables
2
through
5.

The
quantitative
data
for
the
17
target
analytes
have
been
submitted
along
with
all
supporting
quality
control
data
to
Battefle
Columbus
Division
.
for
statistical
analysis.
Characterization
of
additional
chromatographic
peaks
in
the
HRGC/
MS
data
to
identify
other
compounds
of
interest
to
EPA
has
been
initiated
under
a
separate
work
assignment
(
Contract
No.
68­
02­
4252,
Work
Assignment
No.
23).

C.
Semivolatile
Organic
Compounds
An
analytical
method
for
the
broad
scan
analysis
of
human
adipose
tissue
for
semivolatile
organic
compounds
was
identified
and
evaluated.
The
analytical
method
is
based
on
gel
permeation
chromatography
(
GPC),
Florisil
fractionation,
and
HRGC/
MS.
Figure
1
is
a
schematic
of
the
sample
preparation
and
analysis
procedures.

Forty­
six
composite
specimens
were
prepared
from
the
FY82
NHATS
repository
according
to
a
study
design
provided
by
Battelle
Columbus
Division,
the
EPA
Design
and
Deve?
opment
Branch
contractor.
The
composite
specimens
represent
the
nine
U.
S.
census
divisions
stratified
by
three
age
groups
(
0­
14,
15­
44,
and
45
plus).

Quantitative
data
for
organochlorine
pesticides,
PCBs,
chlorobenzenes,
phthalate
esters,
phosphate
triesters,
and
polynuclear
aromatic
hydrocarbons
were
determined
for
each
composite.
Table
6
summarizes
the
incidence
of
detection
of
selected
semivolatile
organic
compounds
and
the
range
of
concentrations
measured
based
on
extractable
lipid
content.
Tables
7
through
10
qualitatively
demonstrate
the
incidence
of
observation
based
on
census
divisions
and
age
group.
The
feasibility
of
determining
other
halogenated
aromatic
compounds,
including
polybrominated
biphenyls,
polychlorinated
terphenyls,
and
polychlorinated
diphenyl
ethers,
using
this
method
was
demonstrated
through
the
analysis
of
spiked
adipose
tissue
samples.

The
samples
representing
the
45­
plus
age
category
were
also
analyzed
for
toxaphene
(
a
complex
mixture
of
polychloroterpenes)
by
HRGC/
MS­
SIM.
Toxaphene
was
qualitatively
identified
in
12
of
the
14
samples
analyzed.
Quantitation
of
toxaphene
was
not
achieved
due
to
the
complexity
of
the
response
but
was
estimated
to
be
less
than
0.10pg/
g.

4
IC
,,
",,
Table
1.
Inc
,
ace
of
Detect
on
of
Target
Volatile
Organ
C
Compounds
in
the
NHATS
FY82
Composite
Specimens
Wet
tissue
Frequency
of
concentration
Compound
observation
(%)
(
ndg)

Chloroform
l,
l,
l­
Trichloroethane
Bromodichlorornethane
Benzene
Tetrachloroethene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,
Z­
Dichlorobenzene
1,4­
Di6hlorobenzene
Xylene
Ethylphenol
76
48
0
96
61
0
0
91
96
96
0
100
9
63
100
100
100
ND
(
Z)
a
­
580
ND
(
17)
­
830
ND
(
21)
ND
(
4)
­
97
NO
(
3)
­
94
ND
(
1)
ND
(
1)
NO
(
1)
­
250
ND
(
1)
­
9
NO
(
2)
­
280
ND
(
1)
8­
350
ND
(
1)
­
8
ND
(
0.1)
­
2
12­
500
18­
1,400
0.4­
400
aND
=
not
detected.
Value
in
parentheses
is
the
estimated
limit
of
detection.
bThe
exact
isomers
were
not
deterrnined.

5
­­

­­

­­

­­
t
Table
2.
Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
Northeast
Census
Region
Census
division:
New
England
Age
group:
0­
14
15­
44
Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Oibromochloromethane
1,1,2­
Trichloroethane
To1
uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
l,
l92,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1,4­
Dichlorobenzene
X~
I
enea
I
Ethylphenol
~
~~
Middle
Atlantic
45+
0­
14
15­
44
45+

++

++

++

++

c­.
.

++

++

++

++

++

++

++

++

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.
aThe
exact
isomers
were
not
determined.

6
­­

­­
­­

­­

­­

­­
­­­­

­­­­
­­­­

­­­­
­­­­

­­­­

­­­­
­­

­­
­­

­­
­­

­­

­­
­­

­­
­­

­­
­­

­­

­­
Table
3.
Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
South
Census
Region
Census
division:
South
At1antic
East
South
Centra?
West
South
Central
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
49
0­
14
15­
44
45+

Compound
Chloroform
++
+++­+++­­+
++

l,
l,
l­
Trichloroethane
­+
+++­+++­­+
­+
­+

Bromodichloromethane
Benzene
++
++++
++++
++
++
++

Tetrachloroethene
++++
­++­++
­+
­+

Dibromochlocomethane
1,1,2­
Trichloroethane
­­­
a­

To1uene
+­++++
+++­++
++
­+

Chlorobenzene
++
++++
­++­++
++
++

Ethylbenzene
++
++++
++++
++
++
++

Bromoform
Styrene
++
++++
++++
++
++
++

l,
l,
Z,
Z­
Tetrachloroethane
­­
e­­­­+
­+
­+

1,2­
Dichlorobenzene
­+
­+­­­­­
a
­+
++
+­

1,4­
Dichlorobenzene
++
++++
++++
++
++
++

xylenea
++
++++
++++
++
++
++

Ethylphenol
++
++++
++++
++
++
++

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.
aThe
exact
isomers
were
not
determined.

7
­­­

­­­
­­­

­­­
­­­

­­­

­­­
­­

­­
­­

­­

­­
D
Table
4.
Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
North
Central
Census
Region
~

Census
division:
.)
East
North
Central
West
North
Central
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+

Compound
Chloroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
Tetrachloroethene
Dib­
romochloromethane
l,
l,
Z­
Trichloroethane
To1
uene
Chlorobenrene
Ethylbenzene
Bromoform
Styrene
1,1,2,2­
Tetrachloroethane
1,2­
Dichlorobenzene
1,4­
Dichlorobenzene
xyl
enea
Ethylphenol
+++
+++
++

­+­­­+
­+

+++
++­++

­++
­++
++

­­
e
+++
+++
++

+++
+++
++

+++
+++
++

+++
+++
++

+­

++­+­+
+

+++
+++
++

+++
+++
++

+++
+++
++

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.
aThe
exact
isomers
were
not
determined.

8
Table
5.
Incidence
of
Detection
of
Volatile
Organic
Compounds
in
Composited
Human
Adipose
Tissue
from
the
West
Census
Region1
Census
division:
Age
group:

Compound
I
I
Ch1oroform
l,
l,
l­
Trichloroethane
Bromodichloromethane
Benzene
I'
Tetrachloroethene
Dibromochloromethane
l,
l,
Z­
Trichloroethane
To1uene
Chlorobenzene
Ethylbenzene
Bromoform
Styrene
R
1
Mountain
Pacific
0­
14
15­
44
45+
0­
14
15­
44
45+

+
+
+
f
+
+

­+
+
+
+
­­
­­

+
+
+
+
+

­
+

+
+

+
+

+
+

­+
i
l,
f,
2,2­
Tetrachloroethane
e
1,2­
Dichlorobenzene
+
+

1,4­
Dichlorobenzene
+
+
+

xylenea
+
+
+

Ethylphenol
+
+
+
+
i
+

I
Note:
A.
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.
a
E
The
exact
isomers
were
not
determined.

9
e
Composite
=
Y82
NHATS
Specimens
(
BCL
Protocol
1
I
Ado
Stoole
Isotope
abeled
Surrogate
Compounds
1
Extroction
­
Tissumizer
1
hi<
Lipid
Removoi
c
rIRGC/
Selective
Detector
Screening
JI
I
I
Specific
Comoound
Closs
*
Florisi'
Froctionotion
i
HRGC/
MS
(
Scanning)
0.01
­
0.
I
/&
gjg
(
PCBs.
OCI
Pesticides.
Etc.
1
*
,

AMCCO
?
X
­
21/
Gloss
Fiber
Florisil
i
I
I
i
I
Figure
1.
Flow
scheme
for
analysis
of
semivolatile
organic
i
compounds
in
human
adipose
tissue.

10
Table
6.
Incidence
of
Detection
of
Target
Semivolatile
Organic
Compounds
in
the
NHATS
FY82
Composite
Specimens
~~
~

Range
of
observed
Frequency
of
lipid
concentration
Compound
observation
(%)
a
(
ng/
g)

Dichlorobenzene
Trichlorobenzene
Naphthalene
Diethyl
phthalate
Tributyl
phosphate
Hexachlorobenzene
fi­
BHC
Phenanthrene
Di­
n­
buty1
phtha1ate
HepTachlor
epoxide
trans­
Nonachlor
p,~'
­
DDE
Dieldrin
p,
p'­
DOT
Butylbenzyl
.
phthalate
­

Triphenyl
phosphate
Di­
n­
octyl
phthalate
M
irex
­
tris(
2­
Ch1oroethyl)
phosphate
Total
PCBs
Trichlorobiphenyl
Tetrach1or0bipheny1
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachlorobiphenyl
0ctach
1orobip
heny1
Nonachlorobiphenyl
Decachlorobiphenyl
aSample
size
=
46
composites.
bND
=
not
detected.
Value
in
parentheses
is
the
estimated
limit
of
9
4
40
42
2
76
87
13
44
67
53
93
31
55
69
36
31
13
2
83
22
53
73
73
53
40
13
7
ND
(
9>
b
­
57
ND
(
9)
­
21
ND
(
9)
­
63
ND
(
10)
­
970
ND
(
44)
­
120
ND
(
12)
­
1,300
.

ND
(
19)
­
570
ND
(
9)
­
24
ND
(
10)
­
1,700
ND
(
10)
­
310
ND
(
18)
­
520
ND
(
9)
­
6,800
ND
(
44)
­
4,100
ND
(
9)
­
540
ND
(
9J
­
1,700
ND
(
18)
­
850
ND
(
9)
­
850
ND
(
9)
­
41
ND
(
35)
­
210
ND
(
15)
­
1,700
ND
(
9)
­
33
ND
(
9)
­
93
ND
(
21)
­
270
ND
(
19)
­
450
NO
(
19)
­
390
ND
(
203
­
320
ND
(
18)
­
300
ND
(
22)
­
150
""

detection.

11
Table
7.
Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
West
Census
Region
Census
division:
Mountain
Pacific
Age
group:
0­
14
15­
44
45+
0­
14
45+

Compound
Dichlorobenzene
Trichlorobenzene
Naphthalene
Diethyl
phthalate
Tributyl
phosphate
Hexachlorobenzene
P­
BHC
Phenanthrene
Di­
n­
buty1
phtha1ate
HepTachlor
epoxide
trans­
Nonachlor
2,
p
''­
DDE
Die1drin
~,
p'
­
DDT
Butvlbenzvl
Dhthalate
Tripheny1­
phosphate
Di­
n­
octyl
phthalate
Mirex
m(
2­
Chloroethyl)
phosphate
Total
PCBs
Trichlorobiphenyl
Tetrachlorobiphenyl
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachlorobiphenyl
Octachlorobiphebyl
Nonachlorobiphenyl
Decachlorobiphenyl
Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

12
­­
­­

­­

­­

­­
­­
­­

­­
­­
­­
I
8
Table
­.
Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
Northeast
Census
RegionI
Census
division:
New
England
Middle
Atlantic
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+
]
I
Compound
8
Dichlorobenzene
Trichlorobenzene
Naphthalene
­+
Diethyl
phthalate
+­
Tributyl
phosphate
Hexachlorobenzene
++

1)
8­
BHC
++
Phenanthrene
+­
Di­
n­
butyl
phthal
ate
++
Hepyach1or
epoxide
++
trans­
Nonachlor
++
p,
p'­
DDE
++
Dieldrin
e
,
e'­
DDT
+­
Butylbenzyl
phthalate
++
Triphenyl
phosphate
­+
Di
­
n­
octyl
phthalate
+­
Mirex
­
tris(
PChloroethy1)
phosphate
Total
PCBs
++
Trich1o
robi
pheny1
Tetrachlorobiphenyl
++
Pentachlorobiphenyl
++
Hexachlorobiphenyl
++
Heptachlorobiphenyl
+­
Octachlorobiphenyl
Nonachlorobiphenyl
Oecachlorobiphenyl
Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the­
compoundwas
not
detected
(
response
less
than
2.5
times
S,").
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

13
­­
­­

­­

­­
­­

­­
­­­

­­­

­­­

­­­
­­­
­­­

­­­
­­­

­­­

­­­

­­­
­­­

­­­
­­

­­

­­

­­
­­

­­
t
Table
9.
Incidence
of
Detection
of
Semivolatile
Organic
Compounds
Determined
in
Composited
Human
Adipose
Tissue
from
the
North
Central
Census
Region
Census
division:
Age
group:

Compound
Dichlorobenzene
Trichlorobenzene
Naphthalene
Diethyl
phthalate
Tributyl
phosphate
Hexachlorobenzene
$­
BHC
Phenanthrene
Di­
n­
butyl
phthalate
Hepxachlor
epoxide
trans­
Nonachjor
D
.
D
'
­
DDE
ZL
Dieldrin
e,
p'­
DDT
Butylbenzyl
phthalate
Triphenyl
phosphate
Di­
n­
octyl
phthalate
Mirex
East
North
Central
West
North
Central
0­
14
15­
44
45+
0­
14
15­
44
45+

­­+
­­+
­
d
+­­++­+

­+­­+­++
­+
++­+++
+­
­+
+++
+++
++
­+
­+
­+­­++
­+
­+
­++
+++
++
­­+
­++
++
++
+++
+++
++
­+­­++
+­
­+
++­+­
++
­+­+++
++
­+
­+­­+­­+
­+­­­+
+­

­
tris(
2­
Chloroethyl)
phosphate
Total
PCBs
+++
+++
++
Trichlorobiphenyl
+++
+­
Tetrachlorobiphenyl
­+­­++
++
Pentachlorobiphenyl
­++
­++
++
Hexachlorobiphenyl
­++
­++
++
Heptachlorobiphenyl
+­­­++
++
Octachlorobiphenyl
+­­­++
++
Nonachlorobiphenyl
+­
Decachlorobiphenyl
­+­

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

14
L
I
Table
10.
Incidence
of
Detection
of
Semivolatile
Organic
Compounds
.
Determined
in
Composited
Human
Adipose
Tissue
from
the
South
Census
Region
Census
division:
South
Atlantic
East
South
Centra?
West
South
Central
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+
0­
14
15­
44
454
Compound
Dichlorobenzene
+

­

Trichlorobenzene
­
Naphthalene
­
Diethyl
phthalate
Tributyl
phosphate
Hexachlorobenzene
+
8­
BHC
+
­
Phenanthrene
Di­
n­
butyl
phthalate
+
HeDTach1or
eDoxide
+
trans­
Nonachlor
+
~,
Q'­
DDE
+
Dieldrin
+
e,
p'
­
ODT
+
Butylbenzyl
phthalate
+
Triphenyl
phosphate
+
Di­
n­
octyl
phthalate
+

­

Mi
rex
­­
tris(
2­
Chloroethyl)
phosphate
Total
PCBs
+
Trichlorobiphenyl
+
Tetrachlorobiphenyl
+
Pentachlorobiphenyl
+
Hexachl
orobi
pheny1
+
Heptachlorobiphenyl
+
Octachlorobiphenyl
+

­

Nonach1orobi
pheny1
­
Decachlorobiphenyl
Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

15
This
study
greatly
advances
the
NHMP's
capability
to
monitor
exposure
to
toxic
organic
chemicals.
The
data
base
for
the
number
of
specific
xenobiotic
organic
compounds
detected
in
adipose
tissue
is
expanded.
Organochlorine
pesticides
and
PCBs
have
previously
been
monitored
through
PGC/
ECD
techniques.
The
HRGC/
MS
method,
however,
provides
an
additional
confidence
level
for
determination
since
identification
is
based
on
matching
both
retention
time
and
mass
spectra.
In
addition,
the
detail
on
PCB
levels
is
expanded
as
a
result
of
identifying
specific
degrees
of
chlorination
(
homologs)
and
providing
quantitation
of
individual
responses.
Previous
analyses
for
PCBs
in
the
NHATS
monitoring
program
based
on
the
PGC/
ECD
method
had
resulted
in
semiquantitative
data
based
on
a
single
response.

The
quantitative
data
for
the
target
analytes
have
been
submitted
along
with
all
supporting
quality
control
data
to
Battelle
Columbus
Division
for
statistical
analysis.
Characterization
of
additional
chromatographic
peaks
in
the
HRGC/
MS
data
to
identify
other
compounds
of
interest
to
EPA
has
been
initSated
under
a
separate
work
assignment
(
Contract
No.
68­
02­
4252,
Work
Assignment
No.
23).

D.
PCDD
and
PCDF
The
sample
preparation
was
completed
using
techniques
that
isolate
the
PCDD
and
PCDF
congeners
from
potential
interferences.
The
isolation
of
the
PCDOs
and
PCDFs
was
achieved
using
carbon­
based
chromatography
columns.
Two
different
carbon
materials
were
used
to
complete
the
analysfs
for
thesfull
range
of
the
tetra­
through
octachloro­
PCDD
and
PCDF
congeners.
HRGC/
MS
operated
in
the
SIM
mode
as
required
to
detect
compound
concentrations
ranging
from
less
than
5
pg/
g
(
for
tetra­
and
pentachloro
congeners)
to
greater
than
1,000
pg/
g
for
the
ostachloro
dibenzo­
e­
dioxin.

Table
11presents
the
frequency
of
detection,
mean
concentration,
and
lipid
concentration
range
of
detection
for
the
tetra­
through
octachloro­
PCDD
and
PCDF
congeners.
.
Tables
12
through
15
present
a
qualitative
summary
for
the
detection
of
PCDD
and
PCDF
by
census
divisions
and
age
groups.

The
data
in
Table
11
indicate
that
the
2,3,7,8­
TCDD
was
detected
in
35
of
the
46
composites
with
an
average
lipid­
adjusted
concentration
of
6.2
k
3.3
pg/
g.
The
average
concentration
of
the
other
PCDD
compounds
ranged
from
33.5
pg/
g
for
pentachlorodibenzo­
e­
dioxin
(
detected
in
9s
of
the
composites)
up
to
554
pg/
g
for
octachlorodibenzo­
E­
dioxin
(
detected
in
100%
of
the
composi
tes).

The
data
demonstrated
some
differences
in
PCDD
levels.
for
the
three
age
groups
evaluated
(
Figure
2).
The
PCDFs
were
generally
detected
less
frequently
and
were
present
at
lower
concentration
than
the
PCDOs.
Obvious
trends
in
the
levels
of
the
PCDF
congeners
with
respect
to
age
were
not
observed.
The
mean
values
for
the
PCDD
and
PCDF
data
from
this
study
are
comparable
to
work
that
has
been
reported
for
other
studies
on
adipose
tissue
samples
from
*
the
United
States
(
Schecter
and
Ryan
1986;
Ryan
1986)
and
Sweden
(
Nygren
et
al.
1985)
(
Figure
3).

16
Table
11.
Lipid­
Adjusted
Concentration
of
PCDD
and
PCDF
in
the
NHATS
FY82
Composite
Specimens
~­

Frequency
of
Mean
concentrationa
Range
of
(
P9/
9)
Compound
detection
(%)
detection
(
pg/
g)

ND
(
1.3) 
­
14
ND
(
1.3)
­
5,000
ND
(
13)
­
620
ND
(
26)
­
1,300
19
­
3,700
,

ND
(
1.3)
­
660
ND
(
1.3)
­
90
ND
(
3.0)
­
60
ND
(
3.5)
­
79
ND
(
1.2)
­
890
,
6.2
f
3.3
43.5
&
46.5
86.9
83.8
102
2
93.5
694
k
355
15.6
k
16.5
36.1
f
20.4
23.5
2
11.6
20.9
f
15.0
73.4
2
134
2,3,7,8­
TCDD
1,2,3,7,8­
PeCDD
HxCDDb
1,2,3,4,7,8,9­
HpCDD
OCDD
2,3,7,8­
TCDF
2,3,4,7,8­
PeCDF
H~
CDF~

1,2,3.,
4,6,7,8­
HpCDF
OCOF
76
91
98
98
100
26
89
72
93
39
ablean
concentration
calculated
using
trace
and
positive
quantifiable
values.
bReference
compounds
not
avai1
ab1e
to
specify
isomers.
 
ND
=
not
detected.
Value
in
parentheses
is
the
estimated
limit
of
detection.

.

17
Table
12.
PCDD
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specimens
from
the
Northeast
Census
Region
Census
division:
New
England
Middle
Atlantic
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+

Compound
ZY3,7,8­
TCDD
*
'+
­+­+­­+

1,
ZY3,7,8­
PeCDD
+
+
­++
++
++

HxCDD
+
+
+
++
++
++

lY2,3,4,7,8,9­
HpCDD
+
+
+
++
++
++

OCDD
+
­
k
+
++
++
++

2,3,7,8­
TCDF
+
­­
+­+­.
~

+

2,3,4,7,8
PeCDF
­+
­++
++
++

HxCDF
­­+
­+
++
++

1,2,3,4,6,7,8­
HpCDF
­+
+
++
++
++

OCDF
­+
+
+­+­+­

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
*
A
negative
(­)
value
'
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

78
I
c.

Table
13.
PCDD
and
PCDF
Oetected
in
the
NHATS
FY82
Composite
Specimens
from
the
West
Census
Region
Census
division:
Mountain
Pacific
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+

Compound
a.

2,3,7,8­
TCDD
*
­+
+
­+
+

1,2,3,7,8­
PeCDD
+
+
T
+
+
+

HxCDD
I,
2,3,4,7,8,9­
HpCDD
OCDD
2,3,7,8­
TCDF
2,3,4,7,8­
PeCDF
HxCDF
1,2,3,4,6,7,8­
HpCDF
OCDF
Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.
­­

­­
­­­­
­­
­­

­­
­­

­­
Table
14.
PCDD
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specimens
from
the
South
Census
Region
Census
divi
sion:
South
Atlantic
East
South
Central
West
South
Central
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+
0­
14
15744
45+

Compound
'
2,3,7,8­
TCDD
++
+­+­+­++
+
++
+­+
+­+

1,2,3,7,8­
PeCDD
++
++­+
+­+­+
++
+­+
++
+

HxCDD
++
++++
++++
+
++
++
+
++
+

1,2,3,4,7,8,9­
HpCDD
++
++++
++++
+
++
++
+.
++
+

OCDD
++
++++
++++
+
++
++
+
++
+

2,3,7,8­
TCDF
­+­­+­­­­­­

2,3,4,7,8­
PeCDF
++
+++­+­+­+
++
+­+
+­+

HxCDF
+­++­­++++
+
++
++
+
+­+

1,2,3,4,6,7,8­
HpCDF
++
++++
+­++
+
++
++
+
++
+

OCDF
++­­+
+­­­

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than'
2.5
times
S/
N
but
less
than
10
times
S/
N)
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

20
­­­

­­­
­­­
Table
15.
PCDD
and
PCDF
Detected
in
the
NHATS
FY82
Composite
Specimens
from
the
North
Central
Census
Region
Census
division:
East
North
Central
West
North
Central
Age
group:
0­
14
15­
44
45+
0­
14
15­
44
45+

Compound
2,3,7,8­
TCDD
.
­+
+++
­++
+
+
++

1,2,3,7,8­
PeCDD
++
+++
­++
+
+
++

HxCDD
++
+++
+++
+
++

1,2,3,4,7,8,9­
HpCDD
++
+++
+++
+
+
++

OCDD
++
+++
+++
+
?
++

2,3,7,8­
TCDF
++
+­­­­­
7
2,3,4,7,8­
PeCDF
++
+++
­++
4­+
++

HxCDF
­+
+++
+++
­­++

1,2,3,4,6,7,8
HpCDF
++
+++
+++
+
+
++

­
OCDF
++
+++
­+­

Note:
A
positive
(+)
value
indicates
the
compound
was
detected
at
a
trace
(
response
greater
than
2.5
times
S/
N
but
less
than
10
times
S/
N)
.
or
positive
quantifiable
level
(
response
greater
than
10
times
S/
N).
A
negative
(­)
value
indicates
the
compound
was
not
detected
(
response
less
than
2.5
times
S/
N).
The
number
of
symbols
for
each
age
group
indicates
the
number
of
composites
analyzed.

21
44
PCDD
from
NHATS
FY82
Composite
Specimens
Wet
Tissue
Concentration
15
­
44
years...

045+
years
tipid
Adjusted
Concentration
t
.."
TCiD
250
1
PCOF
from
NHATS
FY82
Y
.
Composite
Specimens
C
­
E
501
OCDO
n
TCDF
PeCDF
HxCDF
HpCDF
OCDF
Figure
2.
PCDD
and
PCDF
distribution
in
the
general
U.
S.
population
by
age
group.

22
I
I
400
 
s
Figure
3.
Comparison
of
PCDD
and
PCDF
concentration
(
based
on
wet
tissue
weight)
profiles
for
Sweden,
the
general
U.
S.
population,
and
upstate
New
York
(
from
top
to
bottom,
respectively).
(
Source:
Stanley
1986;
Schecter
and
Ryan
1986;
Nygren
et
al.
1985)

23
The
results
of
this
phase
of
the
broad
scan
analysis
program
demonstrate
that
the
EPA
NHATS
program
is
an
effective
vehicle
for
documenting
the
exposure
of
the
general
U.
S.
population
to
PCDDs
and
PCDFs.
The
analysis
of
the
46
composite
samples
prepared
from
the
FY82
NHATS
repository
establishes
the
prevalence
of
the
2,3,7,8,­
substituted
tetra­
through
octachloro­
PCDD
and
PCDF
congeners
in
the
U.
S.
population.

The
quantitative
data
for
the
PCDD
and
PCDF
congeners
presented
in
this
report
have
been
submitted
along
with
all
supporting
quality
control
data
to
the
OTS
Design
and
Development
Branch
contractor,
Battelle
Columbus
Division
for
statistical
analysis.
These
data
will
be
analyzed
to
determine
the
significance
of
differences
in
PCDD
and
PCDF
levels
based
on
major
demographic
factors.

E.
Trace
Elements
The
objective
of
this
task
was
to
provide
EPA/
OTS
with
(
1)
a
preliminary
assessment
of
multielement
analytical
techniques
that
are
applicable
for
determining
trace
elements
in
adipose
tissues
and
(
2)
a
qualitative
assessment
of
the
level
of
the
specific
tissue
elements
that
were
present
in
selected
specimens.

The
analyses
of
nine
selected
adipose
tissue
specimens
from
the
FY82
NHATS
repository
were
completed
using
multielement
techniques
ICP­
AfS
and
NAA.
A
total
of
18
elements
were
detected
using
the
two
techniques
and
the
estimated
tissue
levels
are
reported.
Tables
16
and
17
provide
the
results
generated
by
ICP­
AES
and
NAA
for
the
nine
adipose
tissue
specimens.

Elements
determined
by
ICP­
AES
(
Table
16)
were
aluminum,
boron,
calcium,
iron,
magnesium,
sodium,
phosphorus,
tin,
and
zinc.
The
estimated
detection
limits
for
20
additional
elements
determined
by
ICP­
AES
were
also
reported.
Elements
determined
by
NAA
(
Table
17)
were
bromine,
chlorine,
cobalt,
iron,
iodine,
potassium,
sodium,
rubidium,
selenium,
silver,
and
zinc.
The
estimated
detection
limits
for
56
additional
elements
determined
by
NAA
were
also
reported.
The
results
reported
for
iron,
zinc,
and
sodium
are
comparable
for
the
two
methods.

The
results
of
this
study
are
compared
with
tissue
data
reported
in
a
monograph
prepared
for
the
International
Commission
in
Radiological
Protection
(
ICRP)
(
Snyder
et
al.
1975).
Data
in
the
ICRP
report
are
based
on
multiple
sample
analyses
by
single
element
techniques.
The
ICRP
data
were
generated
in
the
mid­
1950s
through
the
mid­
1960s.
The
data
for
the
FY82
NHATS
specimens
are
generally
comparable
with
the
levels
presented
in
the
ICRP
summary
with
the
exception
of
tin.
Tin
was
detected
at
concentration
levels
estimated
to
range
from
4.6
to
15
pg/
g
in
the
NHATS
specimens
compared
to
0.047
pg/
g
for
the
values
reported
for
the
ICRP
report.'
These
tin
levels
were
generated
by
the
ICP­
AES
analyses
but
were
not
confirmed
by
NAA.

i
24
r\
l
iu
W
m
t­
4
0
N
N
0
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r­
0
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e
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v
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rl
h
N
N
n
cv
N
a)
z
n
n
d
m
iu
b
W
m
0
a3
In
0
0
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d
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0
v
W
m
rl
d
cy
N
n
0
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cu
a3
z
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n
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m
cu
N
W
m
m
e­
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..
r(
0
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&
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0
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cn
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m
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m
d
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n
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N
(
v
N
Q)
ri
4
m
n
In
a
N
0
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a3
h
0
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m
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Qco
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P­

WL
u
v)
0
=
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m
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5
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C
4
W
c
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c
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w
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>
v
c
c
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c
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W
.
C
.
C
a
n
V
v)
VIN
111.
RECOMMENDATIONS
Specific
recommem.
2
ions
based
on
analyte
classifica
ion
are
dis
.
cussed
below.

A.
Volatile
Organic
Compounds
Further
analytical
method
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
(
1.0to
5.0
g),
more
efficient
transfer
of
volatile
organics
onto
the
HRGC
column,
and
further
development
of
the
isotope
dilution
quantitation
technique.
These
modifications
can
possibly
be
achieved
by
using
widebore
HRGC
columns
and/
or
cryofocusing
techniques.
I
The
analytical
method
should
be
modified
to
provide
quantitztive
information
on
compounds
of
greater
volatility
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
80
°
C
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.
8D
I
I
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
had
been
archived
prior
to
analysis
for
up
to
2
yr.
I
I
I
B.
Semivolatile
Organic
Compounds
I
The
analytical
method
should
be
fully
validated
through
additional
intra­
and
interlaboratory
analyses.
This
is
necessary
to
fully
define
the
method's
limitations
[
accuracy,
precision,
limits
of
detection
(
LOD),
and
limits
of
quantitation
(
LOQ)],
and
quality
control
(
QC)
requirements
for
reporting
valid
data.
The
method
LOD
and
LOQ
for
individual
analytes
should
be
determined
experimentally
through
replicate
analysis
of
spiked
tissue
samples.
The
HRGC/
MS
and
PGC/
ECD
methods
should
be
evaluated
using
homogenized
split
samples
to
determine
the
comparability
of
data
for
the
organochlorine
pesticides
and
PCB
data.
This
is
necessary
to
determine
whether
trend
lines
can
be
extended
from
existing
PGC/
ECD
data
from
previous
NHATS
analysis
programs.
B
I
I
Before
proceeding
with
the
validation
and
comparability
studies,
the
analytical
method
should
be
modified
to
include
at
least
two
more
internal
standards
for
quantitation.
Surrogate
compounds
that
will
fractionate
in
the
more
polar
Florisil
fractions
are
needed
to
fully
evaluate
method
performance
on
a
per
sample
basis.
Deuterated
phthalate
esters
that
are
commerciallyc
I
27
available
should
be
considered
as
surrogates
in
.
further
evaluation
of
the
ana
lytical
method.

There
is
a
need
to
establish
sufficient
characterized
reference
Samples
for
continued
broad
scan
analysis
projects
for
use
as
QC
samples.
These
QC
samples
should
be
available
in
quantities
comparable
to
the
20­
9
composited
tissue
samples.
This
type
of
QC
sample
could
be
developed
from
lipid
materials
extracted
from
human
adipose
tissues.
The
lipid
materials
should
be
thoroughly
homogenized
and
the
background
levels
of
semivolatile
organic
analytes
established
through
replicate
analysis.
Once
this
reference
material
has
been
characterized
it
could
be
spiked
with
additional
analytes
for
positive
documentation
of
method
performance.

Additional
method
development
is
needed
to
identify
a
more
expedient
means
of
removing
bulk
lipid
from
the
samples.
The
current
analytical
methodology
although
effective,
requires
considerable
time
and
cost
to
prepare
the
samples.

There
is
a
need
to
develop
HRGC/
selective.
detector
analysis
methods
to
generate
data
for
target
analytes
on
a
routine
basis.
Specifically,
HRGC/
ECD
analysis
of
adipose
tissue
could
supply
EPA/
OTS
with
data
for
chlorobenzenes
organochlorine
pesticides,
and
specific
PCB
isomers.
This
approach
would
require
smaller
sample
sizes
and
result
in
more
expedient
sample
preparation
while
maintaining
the
sensitivity
to
achieve
1­
10ng/
g
(
ppb)
detection
levels.
The
approach
of
HRGC/
selective
detector
analysis
could
also
be
used
to
monitor
phosphate
triesters
on
a
routine
basis.

Some
consideration
should
be
given
to
evaluation
of
alternate
HRGC/
MS
techniques
including
SIM,
negative
chemical
ionization
MS,
and
mass
spectrometry/
mass
spectrometry
(
MS/
MS)
to
lower
detection
limits
and
increase
specificity
for
compound
classes
such
as
organochlorine
pesticides,
polychlorinated
biphenyls,
polybrominated
biphenyls,
polychlorinated
terphenyls,
polychlorinated
diphenyl
ethers,
and
polychlorinated
naphthalenes.

C.
PCDO
and
PCDF
The
methods
described
for
PCDD
and
PCDF
analysis
were
developed
in
conjunction
with
the
HRGC/
MS
broad
scan
analysis
method
for
determination
of
general
semivolatile
organic
compounds
in
human
adipose
tissues.
A
continued
effort
in
following
PCDD
and
PCOF
trends
will
require
that
the
analytical
method
as
described
be
fully
validated
through
intra­
and
interlaboratory
studies.

Certified
standards
other
than
the
2,3,7,8­
TCDD
are
not
currently
available,
It
is
imperative
that
the
additional
2,3,7,8­
substituted
PCDD
and
PCDF
congeners
be
made
available
as
certified
materials
for
future
studies
to
allow
accurate
comparison
of
residue
levels
in
the
general
population.

The
analytical
method
should
be
modified
to
include
additional
c
carbon­
13
'
labeled
internal
standards
to
improve
the
accuracy
of
the
quantitation
of
the
tetra­
through
octachloro
PCDD
and
PCDF.

i
28
.?,
i
The
time
required
for
preparation
of
10­
to
20­
9
tissue
samples
by
the
method
is
time
intensive
as
a
result
of
bulk
lipid
removal
by
GPC.
This
procedure
was
necessary
to
achieve
the
overall
objective
of
the
broad
scan
analysis
program.
However,
future
studies
that
focus
on
PCDD
and
PCDF
levels
.
will
require
the
development
of
more
expedient
sample
preparation
techniques.

0.
Trace
Elements
The
study
compared
ICP­
AES
and
NAA
analysis
for
multielement
determination
in
adipose
tissue.
It
is
recommended
that
the
sensitivity,
selectivity,
and
cost
of
each
analysis
technique
be
considered
with
respect
to
the
trace
elements
of
interest
before
proceeding
with
analysis
of
additional
samples.
The
data
collected
from
this
preliminary
scan
of
metals
in
adipose
tissue
demonstrate
that
ICP­
AES
has
sufficient
sensitivity
to
allow
analysis
of
large
numbers
of
adipose
samples
for
multiple
elements
at
a
reasonable
cost.
However,
modifications
of
the
method
are
necessary
to
lower
the
detection
limits.
These
modifications
should
include
increasing
the
sample
size
and
incorporating
an
acceptable
approach
for
correcting
background
resulting
from
overlapping
spectral
interferences.

NAA
has
the
advantage
of
detecting
some
elements
not
possible
by
ICP­
AES
such
as
the
halogens,
rubidium,
and
cesium.
Although
multie1,
ement
analysis
by
NAA
is
much
more
expensive,
it
may
provide
the
sensitivity
and
specificity
needed
to
identify
elements
of
interest.

One
other
analytical
technique
that
should
be
considered
is
high
temperature
graphite
furnace
atomic
absorption
spectrometry.
This
technique
can
provide
lower
levels
of
detection
but
is
limited
to
single
element
measurements
This
technique
can
be
evaluated
for
elements
of
special
interest.

A
study
of
possible
interest
to
EPA
would
be
the
determination
of
elements
directly
associated
with
the
lipid
materials
rather
than
the
whole
tissue.
This
could
be
accomplished
by
rendering
the
adipose
tissue
followed
by
multielement
analysis
of
the
oily
materials.
Based
on
the
results
of
these
studies
further
evaluation
may
be
necessary
to
determine
speciation
of
elements.

A
national
survey
of
human
adipose
tissue
to
determine
prevalence
of
toxic
trace
elements
will
require
stringent
quality
assurance
practices.
This
will
require
method
validation
for
each
element
of
interest,
development
of
a
representative
reference
material,
and
integration
of
a
minimum
QC
program
that
specifies
the
frequency
of
analysis
of
blanks,
spiked
tissues,
and
reference
materials.
A
representative
reference
materia?
can
be
generated
by
isolating
and
homogenizing
lipid
materials
from
tissues
collected
through
the
NHATS
program.
Repetitive
analysis
of
such
a
reference
material
(
spiked
and
unspiked)
can
provide
the
necessary
data
to
document
method
precision
and
accuracy
for
all
samples
analyzed.

29
IV.
REFERENCES
Lucas
RM,
Pierson
SA,
Myers
DL,
Handy
RW.
1981.
RTI.
National
Human
Adipose
Tissue
Survey
Quality
Assurance
Program
Plan.
Preliminary
Draft.
RTI/
1864/
21­
11.

Mack
GA,
Stanley
3.
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).

Nygren
M,
Hansson
M,
Rappe
C,
Domellof
L,
Hardell
L.
1985.
Analysis
of
polychlorinated
dibenro­
p­
dioxins
and
dibenzofurans
in
adipose
tissue
from
soft­
tissue
sarcoma
patients
and
controls.
189th
National
ACS
Meeting
Symposium
on
Chlorinated
Dioxins
and
Dibenzofurans
in
the
Total
Environment
111,
Miami,
Florida,
1985.
Washington,
DC:
ACS.
25:
160­
163
Paper
No.
55.

Ryan
JJ.
1986.
Variation
of
dioxins
and
furans
in
human
tissues
and
organ
by
country.
Chemosphere
15:
3.585­
1593.

Schecter
A,
Ryan
33.
1986.
Chlorinated
dioxin
and
dibenzofuran
levels
in
human
adipose
tissue
from
exposed
and
control
populations.
In:
Ch1,
orinated
dioxins
and
dibenzofurans
in
perspective.
Rappe
C,
Choudhary
G,
Keith
LH,
eds.
Chelsea,
MI:
Lewis
Publishers,
pp.
51­
66.

Snyder
WS,
Cook
MJ,
Nasset
ES,
Karhausen
LR,
Howells
GP,
liptqn
IH.
1975,
Report
of
the
task
group
on
reference
man.
Elmsford,
NY:
Pergamon
Press.
International
Commission
Radiological
Protection
(
ICRP)
Report
No. 
23.

Stanley
3s.
1986a.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
11:
Volatile
organic
compounds.
EPA
560/
5­
86­
036.

Stanley
35.
1986b.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
111:
Semivolatile
organic
compounds.
EPA
560/
5­
86­
037.

Stanley
JS.
1986~.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
IV:
Polychlorinated
dibenzo­
p­
dioxins
(
PCDDs)
and
polychlorinated
dibenzofurans
(
PCDFs).
EPA­
560/
5­
86­
038.

Stanley
JS.
1985.
MRI.
Analytical
method
for
the
determination
of
semi­
volatile
organic
compounds
in
human
adipose
tissue.
Interim
Report,
Revision
No.
2.
Washington,
DC:
Office
of
Toxic
Substances.
Contract
68­
02­
3938
(
Work
Assignment
8).

Stanl ey
JS,
Boggess
KE,
Onstot
3,
Sack
TM,
Remmers
JC,
Breen
J,
Kutz
FW,
Curra
J,
Robinson
P,
Mack
GA.
1986.
PCDDs
and
PCOFs
in
human
adipose
tissue
from
the
EPA
FY82
NHATS
repository.
Chemosphere
15:
1605­
1612.

Stanley
35,
Stockton
RA.
1986.
Broad
scan
analysis
of
human
adipose
tissue:
Volume
6:
Trace
elements.
EPA­
560/
5­
86­
039.

30
APPENDIX
A
GLOSSARY
OF
TERMS
I
i
31
FY82
HpCDD
HpCDF
HRGC
HxCDD
HxCDF
ICP­
AES
I
CRP
MS
NAA
NHATS
NHMP
OCDD
OCDF
OTS
PCDD
PCDF
PeCDD
PeCDF
SIM
TCDD
TCDF
Fiscal
year
1982
Heptachlorodibenzo­
e­
dioxin
Heptachlorodibenzofuran
High
resolution
gas
chromatography
Hexachlorodibenzo­
e­
dioxin
Hexachlorodibenzofuran
Inductively
coupled
plasma­
atomic
emission
spectroscopy
International
Commission
Radiological
Protection
Mass
spectrometry
Neutron
activation
analysis
National
Human
Adipose
Tissue
Survey
National
Human
Monitoring
Program
Octachlorodibenzo­
p­
dioxin
Octachlorodibenzofuran
Office
of
Toxic
Substances
Polychlorinated
dibenzo­
e­
dioxin
Polychlorinated
dibenzofuran
Pentachlorodibenzo­
p­
dioxin
Pentachlorodibenzofuran
Selected
ion
monitoring
Tetrachlorodibenzo­
p­
dioxin
Tetrachlorodibenzofuran
*
PB87177218*

I
BIN:
M15
04­
23­
99
I
NVO
I
CE
:
763657
SH
I
PTO:
1*
524502PAYMENT:
CSHWORNG
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