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Office of
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BROAD SCAN ANALYSIS OF THE FY82
NATIONAL HUMAN ADIPOSE TISSUE SURVEY
SPECIMENS
VOLUME V - TRACE ELEMENTS
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BROAD SCAN ANALYSIS OF HUMAN ADIPOSE TISSUE
VOLUME V: TRACE ELEMENTS
By
John S. Stanley and Rodney A. Stockton
FINAL REPORT
EPA Prime Contract No. 68-02-4252
MRI Project No. 8821-A01
Prepared for
National Human Monitoring Program
Field Studies Branch (TS-798)
Design and Development Branch
Exposure Evaluation Division
Office of Toxic Substances
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, D.C. 20460
Attn: Ms. Janet Remmers and Mr. Philip Robinson,
Work Assignment Managers
Dr. Joseph Breen and Ms. Cindy Stroup,
Program Managers
U S. Environment;!! Frctsction Agency
Region V, Library
230 Scutn Dearborn Street
Chicago, Illinois 60604
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DISCLAIMER
This document is a preliminary draft. It has not been released
formally by the Office of Toxic Substances, Office of Pesticides and Toxic
Substances, U.S. Environmental Protection Agency. It is being circulated
for comments on its technical merit and policy implications.
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PREFACE
This report is the final document of a five-volume series that de-
tails 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 Sur-
vey (NHATS) fiscal year 1982 (FY82) repository.
This final volume summarizes data generated from the analysis of
selected samples for trace elements using two multielement analysis techni-
ques, inductively coupled plasma-atomic emission spectrometry (ICP-AES) and
neutron activation analysis (NAA). Volume I, the Executive Summary, provides
a synopsis of all analysis efforts completed under the broad scan analysis
program. Volumes II through IV deal specifically with the chemical analysis
of the NHATS composites for general volatile organics, semivolatile organics,
and polychlorinated dibenzo-p_-dioxins (PCDD) and dibenzofurans (PCDF). 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 Develop-
ment Branch contractor, Battelle Columbus Laboratories.
The entire series of reports are references as follows:
Stanley JS. 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 II: Volatile organic compounds. EPA 560/5-8-036.
Stanley JS. 1986. Broad scan analysis of human adipose tissue:
Volume III: 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 poly-
chlorinated dibenzofurans (PCDFs). EPA 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. 68-02-3938 and 68-02-
4252, Work Assignments 8 and 21, respectively, Ms. Janet Remmers, Work Assign-
ment Manager and Dr. Joseph Breem. Project Officer).
The experimental design for selecting samples for trace element analy-
sis and preparing the composite samples from the NHATS repository for the broad
scan analysis of organics was provided by Dr. Gregory Mack, Battelle Columbus
Laboratories, under contract to the EPA/OTS Design and Development Branch
(Mr. Phillip Robinson, Task Manager and Ms. Cindy Stroup, Program Manager).
MIDWEST RESEARCH INSTITUTE
m E. Going Paul C. Constant
frector Program Manager
Chemical Sciences Department
i i i
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TABLE OF CONTENTS
Page
Executive Summary vii
I. Introduction 1
A. Broad Scan Analysis Strategy 1
B. Work Assignment Objective 1
C. Organization of This Report 2
II. Recommendations 2
III. Experimental 3
A. Human Adipose Tissue Samples 3
B. Instrumentation ' 3
1. Inductivity Coupled Plasma-Atomic Emission
Spectrometry 3
2. Neutron Activation Analysis 3
C. Sample Preparation 4
1. Inductively Couple Plasma-Atomic Emisstion
Spectrometry 4
2. Neutron Activation Analysis 4
D. Detection Limits 4
1. Inductively Coupled Plasma-Atomic Emission
Spectrometry 4
2. Neutron Activation Analysis 6
E. Quality Assurance 6
1. Inductively Coupled Plasma-Atomic Emission
Spectrometry 6
2. Neutron Activation Analysis 6
V. Results 6
A. Inductively Coupled Plasma-Atomic Emission
Spectrometry 6
1. Precision 7
2. Accuracy 7
3. Detection Limits 12
B. Neutron Activation Analysis 12
1. Accuracy 12
2. Detection Limits 12
3. NAA Versus ICP-AES Results 12
C. Discussion 20
VI. Quality Assurance/Quality Control 20
VII. References 25
Appendix A - Characteristic Wavelength Scans for Individual Trace
Elements in Blanks (VSTD1), 10 (jg/g Standard (AGHN03,
SSTD3, SSTD4), and Adipose Tissue (Fat, Sample C-l) . . A-l
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LIST OF TABLES
Table
1
2
3
4
5
6
7
8
9
10
Mass of Adipose Tissue Analyzed by NAA
Concentration (ug/g) for Trace Elements in Adipose Tissue
Determined by ICP-AES Analysis . . . . .
Relative Standard Deviation Between Adipose Samples C-l,
C-2 and C-3
Fortified Reagent Blank Recoveries for ICP-AES
NBS Bovine Liver No. 1577A Recoveries for ICP-AES
ICP-AES Method Detection Limits for Human Adipose Tissue . .
Summary of Data for Trace Elements (ug/g) Identified in
Nine Human Adipose Tissue Specimens by NAA
Results of the Neutron Activation Analysis (NAA) for Trace
Elements in the NBS SRM 1577-Bovine Liver
Results of the Neutron Activation Analysis (NAA) for Trace
Elements in the NBS SRM 1570-Spinach
Calculated Detection Limits for Trace Elements from the
Neutron Activation Analysis (NAA) of Nine Adipose Tissue
Soecimens
Page
5
8
9
10
11
13
14
15
16
17
11 Comparison of ICP-AES and NAA Results for Sodium (Na),
Iron (Fe), and Zinc (Zn) in Selected Human Adipose
Tissue Samples 19
12 Comparison of Elements Selected in the NHATS FY82 Specimens
and the ICRP Reference Man 21
13 ICP-AES Analysis of ICS2 Standard 23
14 Y-Internal Standard Recovery 24
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EXECUTIVE SUMMARY
The U. S. Environmental Protection Agency's Office of Toxic Sub-
stances (EPA/OTS) maintains a unique program for monitoring human exposure to
potentially toxic substances through the National Human Adipose Tissue Survey
(NHATS). NHATS is a statistically designed annual program to collect and
analyze a nationwide sample of adipose tissue specimens for toxic compounds.
NHATS focuses on documenting trends in human exposure to environmentally per-
sistent contaminants, specifically, organochlorine pesticides and polychlori-
nated biphenyls (PCBs).
EPA/OTS has recognized a need to expand the use of the NHATS pro-
gram to provide a more comprehensive assessment of toxic substances that
accumulate in adipose tissues. The NHATS specimens collected during fiscal
year 1982 (FY82) were designated for broad scan analysis. This broad scan
analysis was used to detect volatile and semivolatile organic compounds and
trace elements.
This report deals specifically with the measurement of trace ele-
ments in adipose tissue specimens from the FY82 NHATS repository. The objec-
tive of this study 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) provide 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 two multielement techniques: in-
ductively coupled plasma-atomic emission spectroscopy (ICP-AES) and neutron
activation analysis (NAA). A total of 18 elements were detected by the two
techniques. The estimated tissue levels are reported.
Elements determined by ICP-AES were aluminum, boron, calcium, iron,
magnesium, sodium, phosphorus, tin, and zinc. The estimated detection limits
for 20 additional elements determined by ICP-AES are also reported. Elements
determined by NAA were bromine, chlorine, cobalt, iron, iodine, potassium,
sodium, rubidium, selenium, silver, and zinc. The estimated detection limits
for 56 additional elements determined by NAA are 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 Protec-
tion (ICRP) (Snyder, Cook, Nasset, Karhausen, Howells, Tipton 1975). The
data in the ICRP report are based on multiple sample analyses by single ele-
ment 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 ug/g
in the NHATS specimens compared to 0.047 ug/g for the values in the ICRP re-
port. These tin levels were estimated from the ICP-AES analyses but were not
confirmed by NAA.
VI 1
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I. INTRODUCTION
The National Human Adipose Tissue Survey (NHATS) is the main opera-
tive program of the National Human Monitoring Program (NHMP). The NHMP was
first established by the U.S. Public Health Service in 1967 and was subse-
quently transferred to U. S. Environmental Protection Agency (EPA) in 1970.
During 1979 the program was transferred within EPA to the Exposure Evaluation
Division of (EED) 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 com-
pounds. The objective of the NHATS program is to detect and quantify the prev-
alences of toxic compounds in the general U.S. population. The NHATS data
address part of OTS's mandate under 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, Myers, Handy
1981). The survey design ensures that specified geographical regions and demo-
graphic 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 on an annual basis by collect-
ing and chemically analyzing adipose tissue specimens for selected toxic sub-
stances. Historically, organochlorine pesticides and polychlorinated biphenyls
(PCBs) have been the compound of interest.
A. Broad Scan Analysis Strategy
EPA/OTS recognized the need to provide a more comprehensive assess-
ment of the toxic substances that accumulate in adipose tissue. An aggres-
sive strategy to assess TSCA-related substances that persist in the adipose
tissue of the general U.S. population has been developed by EED. The NHATS
specimens collected during fiscal year 1982 (FY82) were selected for a broad
scan analysis of volatile and semivolatile organic TSCA-related chemicals and
tree elements (Mack, Stanley 1984).
B. Work Assignment Objectives
The objective of this phase of broad scan analysis work assignment
was to determine the specific trace elements and the appropriate concentra-
tions in human adipose tissue. The data generated from this study will serve
as a preliminary basis for assessing the appropriateness of using human adi-
pose tissue for monitoring exposure to potentially toxic trace elements.
This report deals specifically with the measurement of trace ele-
ments in selected human adipose tissue samples via two multielemental analy-
sis techniques. Inductively coupled plasma-atomic emission spectrometry
(ICP-AES) and neutron activation analysis (NAA). A computer-assisted litera-
ture review completed before this analysis task showed that there was very
little information on the trace element composition of human adipose tissue.
(Barry 1981; Bryne, Kosta 1978; Casey, Guthrie, Robinson 1982; Gross, Pfitzer,
Yeager, Kehoe 1975; Kowal, Johnson, Kraemer, Pahren 1979; Mangelson, Hill,
Nielson, Eatough, Christensen, Izatt, Richards 1982; Snyder, Cook, Nasset,
Karhausen, Howells, Tipton 1975; Sumino, Hayakawa, Shibata, Kitamura 1975).
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Hence, the results of this task produced valuable information on the levels
of specific trace elements in human adipose tissue.
C. Organization of This Report
Section III of this volume describes the analytical procedures for
the two multielement techniques. Section IV presents the results of the adi-
pose tissue analyses. Section V summarizes the quality control (QC) proce-
dures and analysis results. Section VI is a compilation of the pertinent
references. Appendix A is included to provide examples of the emission re-
sponses observed for inductively coupled plasma-atomic emission spectroscopy
(ICP-AES) wavelength scans characteristic: for each element as measured for a
blank, a calibration standard, and an actual sample.
II. RECOMMENDATIONS
The study reported in this document compares ICP-AES and neutron
activation analysis (NAA) 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 demonstrate that ICP-AES has sufficient sensitivity
to allow analysis of large numbers of adipose samples for multiple elements at
a reasonable cost. However, method modifications are necessary to lower the
detection limits. These modifications include increasing the sample size and
incorporation of 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 multielement
analysis by NAA results in considerably higher costs, it may provide the
necessary sensitivity and specificity for elements of particular interest
to EPA.
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 mea-
surements. 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 would require a methods development effort since metal complexes
will be affected by the acid digestion procedure described in the report. 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 specific 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 quality
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control program that specifies the frequency of analysis of blanks, spiked
tissues, and reference materials. A representative reference material 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 pre-
cision and accuracy for all samples analyzed.
III. EXPERIMENTAL
A. Human Adipose Tissue Samples
The adipose tissue samples were randomly selected from a set of
specimens identified by the EPA Design and Development Branch contractor,
Battelle Columbus Laboratories. Criteria for selecting the nine specific
tissue samples included ample mass for two multielement techniques (greater
than 10 g). The samples were visually checked to verify that the contents
were primarily fatty tissues.
B. Instrumentation
1. Inductively Coupled Plasma-Atomic Emission Spectrometry
The adipose tissues were analyzed using a Jarrell-Ash Model 1155A
inductively coupled argon emission spectrometer at MRI. The analytical oper-
ating conditions were:
Forward Power (kw): 1.15
Reflected Power (w): < 1.0
Observation Height (mm): 18
Nebulizer: Fixed cross-flow
Peristaltic pump
Coolant Gas Flow (L/min): 18
Auxiliary Gas Flow (L/min): 0
Sample Gas Flow (L/min): 0.4
Solution Uptake (mL/min): 1.8
Operation and calibration procedures followed the manufacturer's
guidelines. (Jarrell-Ash Division 1979) A calibration curve was generated
using a 20% (v/v)'nitric acid blank and a 10 (jg/mL multielement standard.
The multielement standard was prepared from commercially available 100 ug/mL
stock (Spex Industries, Edison, New Jersey) in 20% (v/v) nitric acid.
2. Neutron Activation Analysis
The NAA was performed by General Activation Analysis, Inc., in San
Diego, California using 4096 and 8192 channel gamma ray spectrometer systems
equipped with Ge(Li) detectors after irradiation in a TRIGA® Mark 1 reactor.
The very short-lived isotopes were determined 1 min after irradiation at a
flux of 2.5 x 1012 n/cm2s for 1 min. The short-, medium-, and long-lived
isotopes were determined 1 h, 1 day, 1 wk, and 3 wk after irradiation for 30
min at a flux of 1.8 x 1012 n/cm2s.
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C. Sample Preparation
1. Inductively Coupled Plasma-Atomic Emission Spectrometry
Approximately 0.5-g aliquots of the adipose tissue specimens and
associated quality control samples were placed in weighed glass culture tubes
with Teflon@-lined screw-caps. Four milliliters of 50% (v/v) nitric acid
that contained 9.96 (jg of yttrium (Y) was added to each tube. The loosely
capped tubes were allowed to stand at room temperature for 30 min and were
the placed in an oven at 110°C for 1 h. The tubes were removed from the oven
to tighten the caps and then were returned to the oven for 30 min. The diges-
tion tubes were removed from the oven, the caps were loosened to relieve the
pressure, and then were returned to the oven for an additional 30 min. The
tubes were removed from the oven to cool and the samples were diluted with
deionized water (greater than 18 megaohm resistivity) to a weight of approxi-
mately 10 g. The tubes were resealed and returned to the oven for 15 min.
The tubes were removed from the oven, cooled, and the final digestate weights
were measured and recorded.
2. Neutron Activation Analysis
Minimal sample preparation was required. The quantities of adipose
tissue listed in Table 1 were sealed in polyethylene vials, irradiated in the
TRIGA® Mark 1 reactor, and analyzed. Two different aliquots of each sample
were irradiated at varying time spans (1-30 min) to determine the short- and
long-lived isotopes.
D. Detection Limits
1. Inductively Coupled Plasma-Atomic Emission Spectrometry
Detection limits of the ICP-AES were determined by two criteria:
(a) the mean and standard deviation concentrations were calculated for 10
replicate analyses of a quality control adipose sample. Three times the
standard deviations were selected as the method limits of detection for the
element. The adipose sample used for this analysis is identified as sam-
ple C-l and is described with the ICP-AES method quality control procedures
in this report, (b) The quality control adipose sample was scanned across a
2 Angstrom region of the spectrum to determine spectral interferences, which
may result in false values. Interferences were observed for silver, arsenic,
barium, beryllium, cadmium, cobalt, chromium, copper, mercury, potassium,
manganese, molybdenum, nickel, lead, antimony, selenium, titanium,, and thal-
lium. The method limit of detection for each of these elements was calculated
as the highest false positive bias plus three times the standard deviation
determined from the 10 replicate analyses,
Appendix A contains copies of the wavelength scans for all elements.
The x-axis is absolute emission counts. These scans are superimposes on each
plot. These include (1) a calibration blank (VSTD1), (2) a standard equivalent
to 10 (jg/g (AGHN03, VSTD2, SSTD3 or SSTD4), and (3) the observed response for
a quality control adipose sample (C-l).
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Table 1. Mass of Adipose Tissue Analyzed by NAA
Sample mass (grams)
NHATS sample no.
Short irradiation'
Long irradiation
b
8110967
8200586
8201022
8201428
8202046
8202962
8204083
8205874
8206278
NBS liver SRM 1577
NBS spinach SRM 1570
0.6258
1.0450
0.6621
0.7270
0.7679
0.9964
0.8747
0.9221
1.0401
0.2223
0.1989
8.0992
11.4472
11.6512
9.9623
9.9502
10.5311
12.2480
11.3542
11.7879
3.7243
2.8454
Sample irradiated for 1 min for measurement of short-lived radio-
, isotopes.
Sample irradiated for 30 min for measurement of long-lived isotopes.
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2. Neutron Activation Analysis
Method detection limits for the NAA were determined as six times
the standard deviation of the noise level or the concentration required to
generate a photopeak 10% greater than the baseline.
E. Quality Assurance
1. Inductively Coupled Plasma-Atomic Emission Spectrometry
The accuracy of the ICP analysis method was determined by prepara-
tion and analysis of spiked reagent blanks, NBS Spinach No. 1570, NBS Bovine
Liver No. 1577a, and spiked NBS Bovine Liver 1577a. The spiked reagent blanks
and spiked NBS Bovine Liver were prepared by adding approximately 50 ug of
each element to the respective matrix.
Three subsamples (approximately 0.5 g each) of a bulk adipose sample
were prepared by the procedures described for the NHATS specimens and were
analyzed to evaluate the precision of the ICP-AES method. These subsamples
were labeled C-l, C-2, and C-3. These subsamples are referred to as repli-
cates of a single sample. However, no effort was exerted to homogenize the
matrix before subsampling.
An instrument check standard (ICS2) was analyzed every 10th sample
during the analysis of the adipose tissue to monitor the ICP-AES calibration.
The metal concentration of the instrument check standard was equivalent to
0.5 ug/g for each of the elements.
Two complete method blanks were prepared following the procedures
described for the NHATS specimens, although no adipose sample was added to the
nitric acid digestion procedure. The responses observed for the reagent
blanks were used for background contribution corrections with the actual
samples.
An internal standard, yttrium, was added to each digested sample
prior to the ICP-AES digestion procedure to monitor nebulization efficiency.
The amount added was 9.96 ug per sample.
2. Neutron Activation Analysis
The accuracy of NAA was determined by preparation and analysis of
NBS SRMs 1577 (bovine liver) and 1570 (spinach). Empty polyethylene vials
were carried through the irradiation procedure and analysis to document and
correct for background contribution.
IV. RESULTS
A. Inductively Coupled Plasma-Atomic Emission Spectrometry
The results of the ICP-AES analysis for the nine adipose tissues
and the three quality control replicates (C-l, C-2, and C-3) are shown in
Table 2. Only those elements that had concentrations above the estimated
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detection limit for one or more of the samples are listed. Sodium and phos-
phorus were detected in all samples at concentrations of greater than 100
ug/g based on wet tissue weight. Calcium, iron, magnesium, tin, and zinc
were also present in all samples. Aluminum was detected in 7 of the 12 sam-
ples. Boron was detected in only the three quality control bulk adipose
tissue samples.
1. Precision
The triplicate analyses of a bulk adipose tissue sample (C-l, C-2,
and C-3) demonstrated acceptable precision (Table 3) for all elements between
samples except for aluminum and boron. Aluminum was detected in only one of
the three replicates, while boron was detected in all three samples. The range
of relative standard deviations for the analysis ranged from 13% for phosphorus
to 57% for boron.
Table 3 also summarizes the precision of the 10 replicate ICP-AES
analyses of sample C-l. These results demonstrate relative standard devia-
tions ranging from 0.50% for magnesium up to 7.6% for aluminum. Since the
detectable levels of aluminum are essentially a trace value (2.5 x the limit
of detection), this difference in precision might reflect the ICP-AES per-
formance near the detection limit. Based on the precision of the multiple
analyses of sample C-l (Table 3), the variability of the other elements could
have been caused by sample preparation or a lack of homogeneity among the
three subsamples.
2. Accuracy
Table 4 lists recoveries of the selected elements from fortified
reagent blanks. These elements correspond to the analytes detected in the
adipose tissue by ICP-AES. The spike recoveries for these elements ranged
from 89.4 to 119%. The recovery of 119% was determined for iron using a
secondary characteristic emission wavelength at 2714 Angstrom compared to
103% for the response observed at the primary wavelength at 2599 Angstroms.
The values for iron reported in Table 2 were calculated using the primary
characteristic wavelength at 2599 Angstroms.
Table 5 presents additional method accuracy data based on the re-
covery of the same six elements in spiked and unspiked NBS Bovine Liver 1577a.
The accuracy for the ICP-AES analysis of the unspiked liver varied from 80.7%
for iron to 114% for phosphorous compared to certified values. Again, it
should be noted that the accuracy for iron varies from 80.7% at 2714 Angstroms
compared to 90.1% at 2599 Angstroms. Concentration values for tin and boron
were also determined for the bovine liver, although no certified value is
available for comparison. The spike recovery values for the nine elements
added to the certified reference material ranged from 87.2 to 128%. A re-
covery for phosphorous spiked to this sample was not reported since the spike
level equivalent to 100 ug/g was negligible in comparison with the certified
concentration of 11,100 ug/g.
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Table 3. Relative Standard Deviation Between
Adipose Samples C-l, O2 and C-3
Element
Al
B
Ca
o
Fe (2714 A)
o
Fe (2599 A)
Mg
Na
P
Sn
Zn
ocn f°/\^
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C
56
21
32
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19
16
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23
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RSD (%)b
7.6
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0.95
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0.51
0.50
1.3
1.0
2.3
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ncn o/ Standard deviation -,nn ~ ,. ,
RSD % = jj T—r-=— x 100; n = 3 replicates
Mean concentration ' K
b(C-l, C-2, C-3).
Relative deviation of 10 instrumental analyses of
sample C-l.
Not calculated because C-2 and C-3 were below the
detection limit.
-------
Table 4. Fortified Reagent Blank Recoveries for ICP-AES
Element
Al (3082 A)
Al (2373 A)
B
Ca
Fe (2714 A)
Fe (2599 A)
Mg
Na
P
Sn
Zn
Observed concet
Amount of
fortification
(M9)
96.4
96.4
95.6
96.0
95.2
95.2
92.4
92.0
96.0
96.0
96.0
itrations are blank cor
Mean observed
concentration
(Hg/g)
93.9 ± 1.8(s)
95.5 ± 1.7(s)
85.4 ± 2.3(s)
94.5 ± 2.6(s)
114 ± 2(s)
97.9 ± 1.4(s)
104 ± 2(s)
99.8 ± 1.2(s)
90.1 ± 1.8(s)
103 ± l(s)
108 ± l(s)
rected; (s) = standard d
Recovery
97.4
99.0
89.4
98.4
119
103
112
108
93.8
108
112
eviation;
n = 4.
10
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3. Detection Limits
The detection limits for the ICP-AES technique presented in Table 6
are based upon a conservative means of calculation because instrumental back-
ground correction was not used. The detection limits are sufficiently high
to overcome any false bias caused by spectral overlap or background shift.
The incorporation of background correction could lower the detection limits
considerably. In most cases, the background and spectral overlap corrected
detection limits would be in the parts per billion (ng/g) to parts per
million (ug/g) range.
B. Neutron Activation Analysis
Table 7 presents the elements detected by NAA at concentrations
greater than detection limits for each sample. The elements determined by
NAA were bromine, chlorine, cobalt, iron, potassium, sodium, and zinc. These
elements were detected in all nine of the adipose tissue samples. Selenium
and rubidium were detected frequently but not in all specimens. Gold,
silver, and iodine were detected in only one or two specimens.
1. Accuracy
NBS standard reference materials (bovine liver SRM 1577a and spinach
leaves SRM 1570) were analyzed with the nine adipose tissue samples to deter-
mine the accuracy of NAA. The results of the bovine liver analysis and the
percent accuracy results are tabulated in Table 8. The NAA method shows good
accuracy for all elements with reported certified values. The observed con-
centration for cobalt was determined to be 360% greater than the NBS value.
As noted in Table 8, the value reported for cobalt by NBS is not certified.
Although, since the data was provided from a nonreference method or was not
determined by at least two independent methods. The results of the spinach
leaves (SRM 1570) analysis and percent accuracy are tabulated in Table 9.
Again, these results demonstrate good accuracy (91 to 100%) for all elements
except chromium, zinc, thorium, and bromine, which range from 67 to 80% of
the NBS reported values.
2. Detection Limits
The detection limits (Table 10) as calculated by General Activation
Analysis, Inc., depend upon the amount of time between irradiation and analy-
sis and the number and amount of interfering elements. Table 9 provides the
detection limits for an additional 56 elements that were determined by NAA.
3. NAA Versus ICP-AES Results
The results of the NAA analyses for sodium, iron, and zinc are in
agreement with the values reported for the corresponding samples analyzed by
ICP-AES. Table 11 summarizes the data for these three elements as determined
by the two multielement techniques. Differences in the values from the two
analytical procedures might be attributed to inhomogeneity of the adipose
tissue specimens. Concern for introducing contamination deterred any attempt
to homogenize the specimens.
12
-------
Table 6. ICP-AES Method Detection Limits
for Human Adipose Tissue
Element Detection limit (ng/g)a
Ag
Al (3082 A)
o
Al (2373 A)
As
B
Ba
Be
Ca
Cd
Co
Cr
Cu o
Fe (2714 A)
o
Fe (2599 A)
Hg
K
Mg
Mn
Mo
Na
Ni
P
Pb
Sb
Se
Sn
Ti
Tl
Y
Zn
3.1b
0.63
0 78
28 h
0.32°
h
0.28°
0.048
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0.07jjD
0.94°
2-3h
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1.4°
3.2
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h
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0.22
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8.3 ,
n
0.71°
6.6
r- -i U
3.8b
12b
0.36,
h
0.36°
12b
0.22
0.13
The detection limit for a particular element was
calculated as three times the standard deviation
determined from 10 replicate analyses of the QC
.sample (C-l).
The detection limit calculation indicates the
consideration for interferences as determined
from the QC sample (C-l).
13
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Table 8. Results of the Neutron Activation Analysis (NAA)
for Trace Elements in the NBS SRM 1577-Bovine Liver
Element
Potassium, K
Iron, Fe
Zinc, Zn
Rubidium, Rb
Manganese, Mn
Selenium, Se
Chlorine, Cl
Cobalt, Co
Molybdenum, Mo
NBS certified3
concentration
0.97%
270 ± 20 ug/g
130 ± 10 pg/g
18.3 ±1.0 ug/g
10.3 ±1.0 ug/g
1.1+0.1 ug/g
(2,600 ug/g)
(0.18 ug/g)
(3.2 ug/g)
Observed
concentration
0.96%
260 ug/g
140 ug/g
18 ug/g
9.6 ug/g
1.1 ug/g
2,700 ug/g
0.62 ug/g
3.4 ug/g
Percent (%)
accuracy
99
96
110
98
93
100
104
360
106
Values in parentheses are not certified by NBS (information only).
These elements are not certified because data were provided from
nonreference methods, or were not determined by at least two inde-
pendent methods.
15
-------
Table 9. Results of the Neutron Activation Analysis (NAA)
for Trace Elements in the NBS SRM 1570-Spinach
Element
Potassium, K
Iron, Fe
Manganese, Mn
Zinc, Zn
Rubidium, Rb
Chromium, Cr
Thorium, Th
Bromine, Br
Cobalt, Co
Scandium, Sc
NBS certified3
concentration
3.56 ± 0.03%
550 ± 20 Mg/g
165 ± 6 Mg/g
50 ± 2 Mg/g
12.1 ±0.2 ug/g
4.6 ± 0.3 ug/g
0.12 ± 0.03 ug/g
(54 ug/g)
(1.5 ug/g)
(0.16 ug/g)
Observed
concentration
3.2%
530 ug/g
155 Mg/g
40 Mg/g
11 Mg/g
3.4 ug/g
o.os ug/g
42 (jg/g
1.5 Mg/g
o.i5 ng/g
Percent (%)
accuracy
90
96
94
80
91
74
67
78
100
94
aValues in parentheses are not certified by NBS (information only).
These elements are not certified because data were provided from
nonreference methods, or were not determined by at least two inde-
pendent methods.
16
-------
Table 10. Calculated Detection Limits for Trace
Elements from the Neutron Activation Analysis
(NAA) of Nine Adipose Tissue Specimens
Element
Aluminum, Al
Arsenic, As
Barium, Ba
Calcium, Ca
Cadmium, Cd
Cerium, Ce
Chromium, Cr
Cesium, Cs
Copper, Cu
Dysprosium, Dy
Erbium, Er
Europium, Eu
Fluorine, F
Gallium, Ga
Gadolinium, Gd
Germanium, Ge
Hafnium, Hf
Mercury, Hg
Holmium, Ho
Indium, In
Iridium, Ir
Lanthanum, La
Lutetium, Lu
Magnesium, Mg
Manganese, Mn
Molybdenum, Mo
Niobium, Nb
Neodymi urn , Nd
Nickel , Ni
Osmium, Os
Phosphorus, P
Palladium, Pd
Praseodymium, Pr
Platinum, Pt
Rhenium, Re
Rhodium, Rh
Ruthenium, Ru
Sulfur, S
Antimony, Sb
Scandium, Sc
Silicon, Si
Samarium, Sm
Range of calculated
detection limits (ng/g)
2.9-6.7
0.084-1.9
1.5-6.2
110-460
2.7-7.1
0.032-0.12
0.076-0.21
0.010-0.025
10-39
0.43-0.97
3.0-14
0.0081-0.027
180-1,100
1.8-5.9
9.3-26
58-130
0.0071-0.014
0.0001-0.043
0.031-0.072
0.035-0.16
0.00010-0.00030
0.060-0.17
0.0017-0.011
49-280
0.23-0.54
0.75-1,450
62-340
0.15-0.43
2.8-6.2
0.011-0.046
1,900-4,400
1.5-4.4
8.1-25
0.31-0.48
0.0079-0.027
0.083-0.51
0.032-0.076
3,900-17,000
0.013-0.021
0.0009-0.0050
420-960
0.0021-0.0054
17
-------
Table 10 (concluded)
Range of calculated
Element. detection limits (ug/g)a
Strontium, Sr
Tantalum, Ta
Terbium, Tb
Tellurium, Te
Thorium, Th
Tin, Sn
Titanium, Ti
Thallium, Tl
Thulium, Tm
Uranium, U
Vanadium, V
Tungsten, W
Yttrium, Y
Ytterbium, Yb
Zirconium, Zr
17-28
0.010-0.026
0.0028-0.0078
0.21-2.0
0.0035-0.011
1.7-4.4
7.6-42
110-350
0.0065-0.010
0.022-0.045
0.062-0.25
0.22-0.56
1,400-4,400
0.0093-0.017
82-140
Detection levels determined as six times the
standard deviation of the observed noise level
18
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Both analytical techniques are capable of determining the presence
of tin at low ug/g concentrations. Tin was detected in the NHATS specimen by
the ICP-AES method at concentrations ranging from 8.7 to 15 ug/g. However,
these concentrations could not be confirmed by NAA with reported detection
limits ranging from 1.7 to 4.4 ug/g for aliquots of the same adipose tissue
specimens. Clarification of this discrepancy for this element will require
additional effort. No major tin contribution was detected in the method
reagent blanks, and it was anticipated that the NAA method detection limit
may require verification through low level spikes.
C. Discussion
As noted in the introduction, very little information is available
in the literature (Snyder et al. 1975; Sumino et al. 1975; Gross et al. 1975;
Bryne, Kosta 1978; Kowal et al. 1979; Barry 1981; Casey et al. 1982; Mangel son
et al. 1982) regarding the levels of specific elements in human adipose tissue.
The most significant source of information was found in a report prepared for
the International Commission on Radiological Protection (ICRP). (Snyder et
al. 1975) This report summarizes elemental composition based on total body
organ and tissue type for what is referred to as "reference man." The data
presented in that report was taken from several literature sources, much of
which is based on activities completed at the Oak Ridge National Laboratory
and University of Tennessee from the mid 1950s to the mid 1960s. The report
does not specify the analytical procedures used to obtain the data, although
some general references are made to colorimetric, atomic emission, atomic ab-
sorption, and DC-Arc plasma emission techniques.
Table 12 compares the range of concentrations observed for specific
elements from the NHATS specimens in this study to the estimates presented
for "reference man" in the ICRP report (Snyder et al. 1975). The ICRP report
specifies that "reference man" consists of a total mass of 70 kg (~ 150 Ib)
with as much as 21% or 15 kg being adipose tissue. The general term, adipose
tissue, in the ICRP report includes subcutaneous adipose, adipose surrounding
organs such as the kidneys or intestines, and interstitial adipose interspersed
among the cells of an organ and yellow marrow. In general, the data generated
by the two multielement techniques are close to the information presented for
"reference man." The most obvious differences are noted for boron, silver,
and tin.
VI. QUALITY ASSURANCE/QUALITY CONTROL
As discussed in Section III of this volume, several samples were
included to provide estimates of method accuracy and precisions through the
analysis of spikes, replicates, and standard reference materials. The results
of these analyses have been presented in Tables 3, 5, 6, 10, and 11. These
data indicate that the ICP-AES and NAA multielement techniques can accurately
and precisely measure trace elements in human adipose tissues.
20
-------
Table 12. Comparison of Elements Selected in the NHATS FY82 Specimens
and the ICRP Reference Man
Reported concentration (|jg/g)
Element
Aluminum (Al )
Boron (B)
Bromine (Br)
Calcium (Ca)
Chlorine (Cl)
Cobalt (Co)
Gold (Au)
Iodine (I)
Iron (Fe)
Magnesium (Mg)
Phosphorus (P)
Potassium (K)
Rubidium (Rb)
Selenium (Se)
Silver (Ag)
Sodium (Na)
Tin (Sn)
Zinc (Zn)
NHATS FY82 specimens
ND(0.63)-4.3
ND(0.32)-22
0.33-2.4b
15-98
360-1, 500b
0. 034-0. 079b
ND-0.0030b
ND(1.4)-13b
3.0-36.
3.5-26
6.5-25
130-220
52-270b
ND-0.27b
ND-0.056b
ND-0.38
150-540 ,
240-1,200°
4.6-15
1.1-6.0,
1.4-4.5b
ICRP reference man
0.35
0.073
0.43
23
1,200
0.024
< 0.33
c
2.4
20
160
320
c
c
0.0013
510
0.047
1.8
Snyder WS, Cook MJ, Nasset ES, Karhausen LR, Howells GP, Tipton IH.
1975. Report of the task group on reference man. ICRP No. 23,
bPergamon Press, pp. 273-334.
Values from NAA. All other values for the NHATS specimens were
observed by ICP-AES.
No estimate provided.
21
-------
In addition to these quality control checks, additional procedures
monitored the performance of the ICP-AES technique. These quality control
checks included routine analysis of a check standard to monitor calibration
and the inclusion of an internal standard to monitor nebulization efficiency.
An instrumental check standard (ICS2) equivalent to 0.5 pg/g of
each element was analyzed every 10th sample with the adipose tissue. Table
13 presents the results of the calibration check completed after the analysis
of the NHATS specimens. These results demonstrate that the calibration stan-
dard falls outside the ± 5% control limit established from 10 replicates of
the same standard analyzed previous to the adipose tissues. Since this cali-
bration check is outside the control limits, the data should be classified as
estimates.
The recovery of the internal standard, yttrium (Y), from all adipose
tissue samples is presented in Table 14. As noted, the recoveries ranging
from 97 to 112% indicate that no losses were experienced due to the efficiency
of nebulization.
The objective of this study was to provide EPA/OTS with qualitative
information on trace elements present in adipose tissue. Further exposure
studies involving trace element measurements of adipose tissue should require
a stringent protocol to maintain the control limits. Further studies normal-
ize reported concentrations for water content of the tissues. This can be
accomplished either through ashing or lyophilization, although the analyst
must be aware that the more volatile elements may undergo losses with these
techniques.
22
-------
Table 13. ICP-AES Analysis of ICS2 Standard
Element
o
Al (3082 A)
0
Al (2373 A)
As
B
Ba
Be
Ca
Cd
Co
Cr
Cu o
Fe (2714 A)
0
Fe (2599 A)
Hg
Mg
Mn
Mo
Na
Ni
P
Pb
Sb
Se
Sn
Ti
Tl
Y
Zn
Control limit (|jg/g)
0.530-0.586
0.529-0.585
0.502-0.554
0.501-0.553
0.431-0.476
0.458-0.506
0.454-0.502
0.484-0.536
0.455-0.503
0.491-0.543
0.464-0.513
0.943-1.04
0.451-0.499
0.518-0.572
0.468-0.518
0.444-0.490
0.407-0.449
0.473-0.523
0.464-0.513
0.437-0.483
0.514-0.568
0.489-0.541
0.501-0.553
0.476-0.526
0.426-0.470
0.494-0.546
0.433-0.479
0.479-0.529
Measured value (ng/g)
0.686
0.744
0.750
0.509
0.421
0.471
0.432
0.520
0.504
0.572
0.482
1.85
0.460
0.635
0.474
0.455
0.468
0.529
0.517
0.742
0.746
0.597
0.731
0.608
0.426
0.646
0.433
0.536
aThe recommended control limits are ± 5% of the mean concentration of
10 replicate analyses.
23
-------
Table 14. Y-Internal Standard Recovery
Sample
8201022
8201428
8200586
8204083
8202962
8206278
8205874
8202046
8110967
c-i
C-2
C-3
Y-% recovery
104
100
106
97
101
103
102
98
98
105
110
112
a9.96 [jg Y added to all samples.
24
-------
VI. REFERENCES
1. Barry PSI. 1981. Concentrations of lead in the tissues of children.
BR J Ind Med 38:61-71.
2. Bryne AR, Kosta L. 1978. Vanadium in foods and in human body fluids and
tissues. Sci Tot Environ 10:17-30.
3. Casey CE, Guthrie BE, Robinson MF. 1982. Copper, manganese, zinc, and
cadmium in tissues from New Zealanders. Biol Trace Elem Res 4:105-115.
4. Gross SB, Pfitzer EA, Yeager DW, Kehoe RA. 1975. Lead in human tissues.
Toxicol and Appl Pharm 32:638-651.
5. Jarrell-Ash Division. March 1979. Jarrell-Ash Mark III AtomComp Interim
Operator's Manual.
6. Kowal NE, Johnson DE, Kraemer DF, Pahren HR. 1979. Normal levels of
cadmium in diet, urine, blood, and tissues of inhabitants of the United
States. J Toxicol and Environ Health 5:995-1014.
7. Lucas RM, Pierson SA, Myers DL, Handy RW. 1981. National Human Adipose
Tissue Survey Quality Assurance Program Plan. Preliminary draft. RTI/
1864/21-11.
8. Mack GA, Stanley J. 1984. Preliminary strategy on the national human
adipose tissue survey. Washington, DC: Office of Toxic Substances,
Contracts 68-01-6721 (Task 21) and 68-02-3938 (Work Assignment 8).
9. Sumino K, Hayakawa K, Shibata T, Kitamura S. 1975. Heavy metals in nor-
mal Japanese tissue. Arch Environ Health 30:487-494.
10. Snyder WS, Cook MJ, Nasset ES, Karhausen LR, Howells GP, Tipton IH. 1975.
ICRP. Report of the task group on reference man. Elmsford, NY Pergamon
Press. International Commission Radiological Protection (ICRP) Report
No. 23.
11. Stanley JS. 1986a. Broad scan analysis of human adipose tissue:
Volume I: Executive summary. EPA 560/5-86-035.
12. Stanley JS. 1986b. Broad scan analysis of human adipose tissue:
Volume II: Volatile organic compounds. EPA 560/5-86-036.
13. Stanley JS. 1986c. Broad scan analysis of human adipose tissue:
Volume III: Semivolatile organic compounds. EPA 560/5-86-037.
14. Stanley JS. 1986d. Broad scan analysis of human adipose tissue:
Volume IV: Polychlorinated dibenzo-p-dioxins (PCDDs) and polychlor-
inated dibenzofurans (PCDFs). EPA 560/5-86-38.
25
-------
APPENDIX A
CHARACTERISTIC WAVELENGTH SCANS FOR INDIVIDUAL TRACE ELEMENTS IN
BLANKS (VSTD1), 10 ng/g STANDARD (AGHNQ3, SSTD3, SSTD4), AND
ADIPOSE TISSUE (FAT, SAMPLE C-l)
A-l
-------
B VSTD1
WAVELENGTH SCANS FOR AG AT 3280 ANGSTROMS
AGHN03 X FAT
INTENSITY
2 0 00.+
1600*
; 0 0 -
a r, n
33S3SS3
X
BBBBBPBSPBBBBBBBBBBBBBPPBBBBBBBBPPBBBBPBBBBBBePBBBBBBBBBBBStfBBB
0 -10
IS AT POSITION
0 -f 1 0
HMLF-UIDTH is i:
A-2
20
-------
VSTD1
INTENSITY
1000*+
800, +
400*
200,+
WAVELENGTH SCANS FOR AG AT 3280 ANGSTROMS
3 AGHN03 X FAT
SSSi
ssss
3SS
: :< x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x x. x x x x x x x x x x x x x x x x x \ x x ,
•.BBBBBBBBEBBBBBBBBBBBBBBBBBBPEBBBBBBBBBPBBBBBBBBBSBPEPFBBEBBBBEB
-20 -10 0 +10
PEAK IS AT POSITION 1 HALF-WIDTH IS 12
A-3
4- 7 0
-------
WAVELENGTH SCANS FOR AL AT 3032 ANGSTROMS
B VSTDl 3 SSTD3 X FAT
INTENSITY
10000,+
i 7
» "7
i 3 3 X
;33XX
X 333
Y
X
XXXX 2
; yss xxx x;< xx 33
.; rB BBS XX XXX
- B 6 t X X X X X X X X X X X ' X X X X • X >' X / X X X X ,
: B B B B B B B
: L;: B B B B B B B F B B B B B B B E B B B B B B ? B B B B B P B B B B B B P B E B B B B £•' B
PEA;-, IS AT POSITION 0 HALF-WIDTH IS il
A-4
-------
WAVELENGTH SCANS FOR AL AT 3032 ANGSTROMS
B VSTD1 3 SSTD3 X FAT
INTENSITY
6000,+
4300,
3600,
2400
.200
3
3X3
3 X
3
X
X3
3
X
3
X
X 3
33
3
3X X 3
33X
;xx x 3
( X XXXXXX 3
EBB X XX X 33
B BB XX XX 33333 333
B B XX 333333333 X
BB B XXXXXXXXXXXXXXXXXXXX XXX
B B
BBB BB
BBB BBBBBBBBBBBBBBB
BBBBBBBBBBBBBBBBBBBBBBBBBBB
30
r
-30
r
-20
T
-10
T
Q
+ 10
+ 20 +
PEAK IS AT POSITION
0 HALF-WIDTH IS 11
A-5
-------
WAVELENGTH SCANS FOR AL AT 2373 ANGSTROMS
B VSTD1 3 SSTD3 X FAT
INTENSITY
12000,+
9600*
200,
1800.
2400,
3 3
TT
w
3 XXX
3 XX X
X X
3 XX
3 33 X
33 333 X
33333333333333 XXXXXXXXXX X
XXXXXXXXXXXXXXXXXXXXX XXXX X
xxxxxxxxx
X 3
XXXX
BB B BBBBBBBBBBB BBB BBBBBBBBB BB B B BB BB
B BB B B BB BBBBBB BBBBBBBBBBBB BBB B
-30
•20
-10
0
+ 10
+ 20
+ 30
PEAK IS AT POSITION 20 HALF-WIDTH IS 10
A-6
-------
E VSTDl
WAVELENGTH SCANS FOR AS AT 1936 ANGSTROMS
4 SSTD4 X FAT
INTENSITY
:. 700* +
2160»+
1520 .
I ,", PA 4.
.4. W L.' >/ V
i40.
X
X 4
XX X XX XXX
XX X XXXX XXXX XX
XXXX XX 4 XXXXXXXX XXX
XX XXXX 4XXXXXX
M4 XXX XXXXX 4
44 X 4 44 444444444
4 44 4444444 444
44 444
444 444
44444
3 B
0.— + -•
-30
B BBBBBB B
-20 -10 0 +10
PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-7
+ 20
+ 30
-------
B VSTD1
INTENSITY
1500,-
WAVELENGTH SCANS FOR AS AT 1936 ANGSTROMS
4 SSTD4 X FAT
1200,
900,
600,
300,+
X
X
X X XXXX XXXX
X XX X X XX X
X X X X XX
XXXX XXX XX
X XXXXXX4X XX 4 X
X XXXX
XXX XX 4
44 X XXXX
4 X 44 444
4 4 444 444
4 44 44444-14 444
4 4
4 44
4 44
44 4
44444
BBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBB
_.!.«...__._____ A.-. — .-. « — -. — — — J — J J — _ _ ._ -L _ __ _ 4. __
TT 1 i T T T
-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-8
-------
B VSTD1
WAVELENGTH SCANS FOR B AT 2496 ANGSTROMS
4 S3TD4 X FAT
.NTENSITY
9S50.+
"7S80.-1-
5 9 10 . +
3940,+
i?70,-L
4 4
XXXX 4
44 XXXX XXXX 44
4444444 4 44444444 XXXX XXXXXXX 4444444444444444
-30 -20 -10 0 +10
PEAK IS AT POSITION 1 HALF-WIDTH IS 12
+ 20
+ 30
A-9
-------
B VSTD1
INTENSITY
4000.+
3200,+
WAVELENGTH SCANS FOR B AT 2496 ANGSTROMS
4 SSTD4 X FAT
1600,+
800,+
xxxxxx
X XX 4
XX X 4
X XX 4
X XXX 444
444444444444444 XXX XXXX 444444444444
XXXXXXXXXXXXXXXXXXXXX XXXXXXXX XX
444
-30 -20 -10
PEAK IS AT POSITION
0
+ 10
+ 20
+ 30
1 HALF-WIDTH IS 12
A-10
-------
WAVELENGTH SCANS FOR BA AT 4934 ANGSTROMS
B VSTDl 2 VSTD2 X FAT
P. A fi r\ . -'-
6400,+
4800,+
3200,+
1600.+
* O^9O OOO
0__J___.___-___,_____L_ — — — — — -- — — X — —. — — — — — _ _. J_ —._.— —,_.-._-.._ J_ _ ™ ._ ™,__-»™ .-J__ -.™____A.
+ T T T T r T ——.--—— ^.—
-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 1 HALF-WIDTH IS 11
A-ll
-------
WAVELENGTH SCANS FOR BE AT 2348 ANGSTROMS
B VSTD1 3 SSTD3 X FAT
INTENSITY
^5000, f
44000,+
2000 , +
22000,+
11000,+
4
1
-30
33
33333
+ _i r
™ T T
-20 -10 0
•7
3
33
33
+ t
— ~* T ""
+10 +20
+ 30
A-12
-------
WAVELENGTH SCANS FOR BE AT 2348 ANGSTROMS
VSTD1 3 SSTD3 X FAT
INTENSITY
25000, +
20000*+
15000.+
ICOOO.-f
5000,+
4
*
t
*
I
I
-30
333
33333
-20
3
333
"~
-10
0
3
3
3
3333
+ -_ — _-—. _L -»
T
+10 +20
+ 30
A-13
-------
WAVELENGTH SCANS FOR CA AT 3968 ANGSTROMS
B VSTD1 2 V3TD2 X FAT
INTENSITY
6233,+
XX
2 X
1680*+ ,X 2
X
2 * X
3122,+
6,
1564.+
t X 2
X 2
;
*
*
i j
T 1
-30 -20
X
2
2
+ i
T
-10 0
X
X 2
XX22
+ 10
4. —
T
+ 20
L
T
+ 30
PEAK IS AT POSITION 2 HALF-WIDTH IS 10
A-14
-------
WAVELENGTH SCANS FOR CD AT 2288 ANGSTROMS
B VSTD1 2 'v'STIC X FAT
INTENSITY
4000,+
3200*
2400,+
1600,+
300,+
: 22 xxxxxxxxxxxxx 22 xxxxxx
:XXXXXXXX2222222XXXXXXXXXXXXXX XXXXX222222XXXX
0_ L_________4._.™________J__ „___ _. L _ _____ _ __L.». __.»„_„-. — — X — — — — — — — — — 4.—
* T T — — -j- — — — — — j. — — — — — _^.™_. ™— T T
-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-15
-------
e VSTDI
INTENGITf
LOOO.+
800,
600,
400,
200,+
WAVELENGTH SCANS FOR CD AT 2288 ANGSTROMS
2 VSTD2 X FAT
2 XXX XXXX
XXX XX 2
XXX 2 XX XXX XX 2 XX
X XXXXXXXXX2XX XXXXXXXX XX 2 XXX
22 XXX2XX
xxxxx
BBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBfcBBBBBBBBBBBBBBBBBBBBBBBBBBBB
0.--+--
-30
•- + --
-20
•- + --
-10
0
, » J. » _
+ 10
+ 20
. _ J. _
+ 30
PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-16
-------
B VSTD1
INTENSITY
550,+
440,
r,30.
220 ,
110.
WAVELENGTH SCANS FOR CD AT 2288 ANGSTROMS
2 VSTD2 X FAT
XX
X XX
2 XX X
X XX 2
2 X XX X
XX XX
X XX XXXXXXXXXXXXXX X 2 )
XXXXXXX 2 X 2 XX
2 XXXXXXXX
O T
X XXX
X
BBBBBBB BBBBB B BB BBBBBBBBBBBBBBBBBBBBBB B B BBBB
B BB B BBBB BBBB BBBBB BBB
f\ i _. _ JL „ _— _ —. J. —__ __-L___ — _-. — _ _ X — «-.-. — — _. — — 4.— — -.-. — -. — -. — 4.—
'J* 1 " T ' T T T T T
-30 -20 -10 0 -HO +20 +30
PEAK IS AT POSITION
1 HALF-WIDTH IS 10
A-17
-------
USTD1
WAVELENGTH SCANS FOR CD AT 2286 ANGSTROMS
VSTD2 X FAT
INTENSITY
3500,+
6BOO.
5100,
3400,
1700,
XXXXXX2XXXXX XXXXXXXXXXXXXXXXX X
XXXXX XXXXXXXXX 2 XXX 2 XXXXXXXXXXXXX
XXX 222 22
BBBBBBB B BBBBBBB BBBBB222BB222222222222
-- + -•
-30
-20 -10 0 +10
PEAK 13 AT POSITION 2 HALF-WIDTH IS 11
A-18
+ 20
+ 30
-------
B V S T D i
WAVELENGTH SCANS FOF: CO AT 2286 ANGSTROMS
2 VSTD2 X FAT
INTENSITY
2500. +
2000,
1500,
1000,
00,
xxxx
XX 2 XX XXXXXXXXX
XX X XXXXX XX
X XXXX 2 XX
XX XX XXXXX
XX XXX 2 XXXXX
XXXXXXXXX
2 2
&BBBBBBB&&BBB&B&BBBB&BBBBBBBBBBBBB&BBBBBBBBB&B&BBBB&BBB&BBB&BBB
0,— + --
-30
. ~. 4. «. .
-10
_1 _ .
f 10
-20 -10 0
PEAK IS AT POSITION 2 HALF-WIDTH IS 11
A-19
•f20
f30
-------
B VSTD1
[NTENSITY
L3000.+
14400,
10SOO,
'200,
3600 ,
WAVELENGTH SCANS FOR CR AT 2677 ANGSTROMS
4 SSTD4 X FAT
44
444
444
44444
44
44
44
4444
44444
44
.\xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
0— — J-—. — —. — _ _. -. _ J- _ « _. _____ __X — —. — ____X_ — — _._ — — — — i — — — — — — — — — X — — — — -. — — — — i-_
^ _ —j — I — 1— — — — _-. — — — ^ — — f. — -J — -[- —
-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 0 HALF-UEDTH IS 12
A-20
-------
B VSTD1
WAVELENGTH SCANS FOR CU AT 3247 ANGSTROMS
2 VSTD2 X FAT
INTENSITY
•7500. +
6000,+
4500,+
3000,+
1500,+
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx;
X ~ «. _, X — — — — — — — — — X — — — — — — — — — X — — — — — — — — — X — — — — — — — — — X — — —
* T T -f. — — — — — — — -j- — — —— f- ^-
-30 -20 -10 0 +10 +?0
PEAK IS AT POSITION 1 HALF-WIDTH IS 11
A-21
+ 30
-------
WAVELENGTH SCANS FOR FE AT 2714 ANGSTROMS
B VSTD1 3 SSTD3 X FAT
INTENSITY
1142,+ 3
3 3
T'56 »
370*
333
3 3
33
33
3333333
XXX
XX XX
X X
X XX
X X
XX XX
333
xxxxxxxx xxxx
xxxxxxxxxxx
33333333333333
33
X X
XX X
XXXX XXXXXX XXX
xxxx
177.-- +
-30
-20 -10 0 +10
PEAK IS AT POSITION 1 HALF-WIDTH IS 12
A-22
+ 20
-f-
+ 30
-------
WAVELENGTH SCANS FOR FE AT 2599 ANGSTROMS
B VSTD1 3 SSTD3 X FAT
INTENSITY
62681,+
50197.J-
37712*
.2743.
X
XXX 3
XXXXX 3
X X
3 X X
3 X X 3
w A A \i
333 X XX 33
_ — J_ _ — _ ___ _ __ L™. __ _—— .— —X— — — _.__— ._.!..— — _ — — _ — — — X _ —__ — — ,
+ i -- 1 -- ------ T -------- T -- T ^
-30 -20 -10 0 +10
1—
+ 20
+ 30
PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-23
-------
B VSTD1
INTENSITY
? i> 00,+
WAVELENGTH SCANS FOR HG AT 1942 ANGSTROMS
4 SSTD4 X FAT
7200,
400,
3600 *
1800.
4 444
444444XXXXXXXXXXXX4XXXXXXXXXXXXXXXXXXXXXXXXXX44444 XXXXX
444444444444 4444444444444
0,
-30
•- + --
-20
•- + --
-10
• + -
0
+ 10
PEAK IS AT POSITION 0 HALF-WIDTH IS 11
A-24
_ J. — _
+ 20
+ 30
-------
B VSTDi
WAVELENGTH SCANS FOR HG AT 1942 ANGSTROMS
4 SSTD4 X FAT
INTENSITY
5000, t
ISOO.T
1 2 0 0 , 4-
4
4
4 4
XXXX XXX X XXX4
400.+X XXXXXXX 4 XX X X XXXXXXXXXXXX X44 X
444444 XXXXXXXXX X 44 XXXX
44 4 44 444XXXXX 4444
4444444 444444
BBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBB
0* 1" 1 1 ~ 1 'I ' r ' H
-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 0 HALF-WIDTH IS 11
A-25
-------
B YSTD1
INTENSITY
1481 ,+
1232,
982 ,
733,
483,
WAVELENGTH SCANS FOR K AT 7664 ANGSTROMS
2 VSTD2 X FAT
XX
90
00
XXXX
XX XXXXXX
XXX
XX
2X
X
X
o
XX 2
XX 2 XX
XXX XXX
XX2 XX
2X
X
X 2
XX
XX
xxxxxxxxxxx
BBB
BB BBBBB BBBB
BBBBBBBBBBBBBBBB BB B
234,— + --
-30
•20
-10
0
•HO
+ 20
— 4. —
+ 30
PEAK IS AT POSITION 3 HALF-WIDTH IS 25
A-2 6
-------
B VSTB1
WAVELENGTH SCANS FOR MO AT 2795 ANGSTROMS
2 VSTD2 X FAT
INTENSITY
28000.+
22400,+
16800,
11200,
5600,+
X
XX X
2 X X 2
X X
2X
22X
X 2
X 2
X 2
0,--+--
-30
-20 -10 0 +^0
PEAK IS AT POSITION 1 HALF-WIDTH IS 11
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+ 30
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VSTD1
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12000,+
9600,+
7200,+
4300,
2400,
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2 VSTD2 X FAT
"3 T>
-20 -10
PEAK IS AT POSITION
+ — — — — — — — _4-_—. — _ — -
I
0 +10
1 HALF-WIDTH IS 10
A-28
+ 20
+ 30
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B VSTD1
WAVELENGTH SCANS FOR MO AT 2020 ANGSTROMS
3 SSTD3 X FAT
INTENSITY
21338, +
17084.
12830,
4321 .
A "7
/ t —
3 3
33 333333333333
333333333333333333333XXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXX333333333
-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 2 HALF-WIDTH IS 11
A-29
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v ;> i LI 1
WAVELENGTH SCANS FOR MO AT 2020 ANGSTROMS
X !- A r
INTENSITY
.2000.+
9600, +
7200. +
I400,
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-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 2 HALF-WIDTH IS 11
A-30
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VSTD1
INTENSITY
2000. +
WAVELENGTH SCANS FOR MO AT 2020 ANGSTROMS
SSTD3 X FAT
1605,+
1210,
815.
420,
33 3
333 333 3
333 XXXX 33
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33 XX
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PEAK IS AT POSITION 2 HALF-WIDTH IS 11
A-31
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B VSTD1
INTENSITY
24623.+
19744.
14S64,
9985,
5105.+
WAVELENGTH SCANS FOR NA AT 5890 ANGSTROMS
3 SSTD3 X FAT
3 3
3 3
X 3
X 3
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226.--+--
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PEAK IS AT POSITION 3 HALF-WIDTH IS 12
A-3 2
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VSTD1
INTENSITY
9500.+
7600.
5700,
3800,
1900.
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3 SSTD3 X FAT
3 33333
3 333 XXXXXXXXXXXXX33333
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-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION
0 HALF-WIDTH IS 10
A-33
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B VSTD1
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4 SSTD4 X FAT
INTENSIFY
5000.+
1000,
3000,
4
4 X
4 X
X
! 0 0 0 ,
4
4 X
4 X
444 X
4444 X
44444 X
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-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION -2 HALF-WIDTH IS 16
A-34
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B VSTD1
INTENSIFY
6676,+
5369,
4062.
2756,
1449,+
WAVELENGTH SCANS FOR P AT 2149 ANGSTROMS
4 SSTD4 X FAT
X
X X
X
44 X
4
4
X 4
4 X
X 4
4
4
4
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4
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4 X
4 X
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-20 -10 0 +10
PEAK IS AT POSITION -2 HALF-WIDTH IS 16
A-35
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+ 30
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2 VSTD2 X FAT
INTENSITY
2800,+
2240,+
1680,+
1120,
560.+
XXX
XX
2 X X
X X
X X
2 X
XXXXXXXX
XX
X
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-30
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-20
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PEAK IS AT POSITION 1 HALF-WIDTH IS
+ 20
+ 30
A-36
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VSTD1
INTENSITY
11000.+
SSOO.
6600.
4400.
2200.
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3 SSTD3 X FAT
3 3
XX333 333 XXXXXXXXXXXX 3/>3?3333333333333X
3333 X 3333333333XXXX XXXXXXXXXXXXXXXX X 3333
B
BBBBBBBBBBBBBBBBBBBBBBBB BBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBBB
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-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION
0 HALF-WIDTH IS 10
A-37
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B VSTD1
WAVELENGTH SCANS FOR SB AT 2068 ANGSTROMS
3 SSTD3 X FAT
INTENSITY
4250.+
3400.
2550.
1700.
3 3
3 X XXXXXX 333 3
850. X333333 3XX XXX X XXX 33333XXX3X333333X3X
33 333 XX3X X XXXX XXXXXX 3 3X
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B
0.--+--
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-20 -10 0 +10
PEAK IS AT POSITION 0 HALF-WIDTH IS 10
+ 20
+ 30
A-38
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10233.+
3214*
6196,
4177.
o i c;g
i- J. ij 7 *
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4 SSTD4 X FAT
4
4 4
XXXX
4
X 4
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X
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X 44444 4 44444
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4 X
XX
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-30
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-20 -10 0 +10 +20
+30
PEAK IS AT POSITION
1 HALF-WIDTH IS 10
A-39
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INTENSITY
£ £ 4 S , +
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4 SSTD4 X FAT
4
4
4 4
•''I AT 1899 ANGSTROMS
4 XXXXXXXXX 4
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4 44444444444XXXX 44444 XXXXX44444
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30
-30 -20 -10 0 -MO
PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-40
— 4. — _
+ 20
+ 30
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VSTD1
INTENSITY
2000.+
1600.+
WAVELENGTH SCANS FOR SM AT 1899 ANGSTROMS
4 SSTD4 X FAT
1200,
300.
xxxxx
XX
XX
XXXXX 4 >
400, X 4444XXX 4 X
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PEAK IS AT POSITION 1 HALF-WIDTH IS 10
A-41
BBBBBBBB
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+20 +30
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VSTD1
INTENSITY
32000.+
25600. +
19200,+
128QG,A
6400,+
WAVELENGTH SCANS FOR TI AT 3349 ANGSTROMS
3 SSTD3 X FAT
3 3
3 33 3
3 3
3 3
3 3
3 3
333 3333
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PEAK IS AT POSITION 0 HALF-WIDTH IS 11
A-42
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B VSTD1
INTENSITY
10000, +
3000.
6000,
4000,
2000,
WAVELENGTH SCANS FOR TL AT 1908 ANGSTROMS
4 SSTD4 X FAT
44
4,
44 XXXXX X 4 XXXX X
X444444XX XXX X XXXXXX4444XX X XX
XXXX4444X XXXX XXX 444444444
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44
0,--+
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A-43
... — •„,,—..... _ .1. —
+30
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VSTD1
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5000,+
4000.+
5000. +
,2000.+
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4 SSTD4 X FAF
4444
X44XXXXXX
X44X XXX
XXXX44 X
XX XX X 4 XXXX X
XX XX X4X XXX X
X XXXX X444 XX
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o +10
2 HALF-WIDTH IS 18
A-44
-30 -20 -10
PEAK IS AF POSITION
+20
+30
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B VSTD1 3 SSTD3 X FAT
INTENSITY
15000,+
12000*+
9000.
6000,
3000,
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33 XX XX 3
33 X 3
33 X X 33
3333 X X 333
33333333 X X 3333
33 XX 3333333
XX 3
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0___L_______ __.i._ — — — — _ _ « J. _ — ______ _.L-._____ — — — J_ — —. _——____ -L _ — — — — _ _ _ _ .L »
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-30 -20 -10 0 +10 +20 +30
PEAK IS AT POSITION 0 HALF-WIDTH IS 12
A-45
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B VSTD1
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2 VSTD2 X FAT
INTENSITY
17000,+
13600,
10200.
6300,+
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XXX XXXXX
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A-46
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TECHNICAL REPORT DATA
(Plccse read Inunctions on the reverse before completing)
1 SePORT NO.
EPA-560/5-86-039
3. RECIPIENT'S ACCESSIOf*NO.
4. TITLH AND SUBTITLE
Broad Scan Analysis of Human Adipose Tissue
Volume 5 - Trace Elements
5. REPORT DATE
December 1986
6. PERFORMING ORGANIZATION CODE
Midwest Research Institute
7. AUTHOR(S)
John S. Stanley and Rodney A. Stockton
8. PERFORMING ORGANIZATION REPORT NO,
8821-A(01)
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Midwest Research Institute
425 Volker Boulevard
Kansas City, Missouri 64110
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-02-3938
68-02-4252
12. SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of To-xic Substances
Field Studies Branch (TS-798)
Desi ^Development Branch/Exposure Evaluation Division
shine
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
J. Remmers and P. Robinson, Work Assignment Managers
J. Breen and C. Stroup, Program Managers
16. ABSTRACT
The U.S. EPA's Office of Toxic Substances (OTS) maintains a unique capability
for monitoring human exposure to potentially toxic substances through the National Human
Adipose Tissue Survey (NHATS). NHATS is a statistically designed annual program to col
lect 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 environ-
mentally persistent contaminants, specifically, organochlorine pesticides and poly-
chlorinated biphenyls (PCBs). The NHATS specimens collected during fiscal year 1982
were designated for broad scan analysis. This broad scan analysis concept was applied
to the determination of trace elements.
This report deals with the measurement of trace elements in selected adipose
tissue specimen from the FY82 NHATS repository. The analyses of nine selected adipose
tissue specimens from the FY82 NHATS repository were completed using two multielement
techniques: inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and neu-
tron activation analysis (NAA). A total of 18 elements were detected using the two
techniques and the estimated tissue levels are reported.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
COSATl Field/Croup
Human Adipose Tissue
Trace Elements
Neutron Activation Analysis (NAA)
Inductively-coupled plasma-atomic emission
Spectroscopy (ICP-AES)
Analysis
Determination
3. 2I5TPI3UT:GN STATE.V1e.NT
Release unlimited
19. SECURITY CLASS ITnu Report)
Unclassified
121. NO. OF PAGES
20. SECURITY CLASS
Unclassified
22. PRICE
EPA Form 2220-I (R«». 4_77) previous EDITION i s OBSOLETE
A-47
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