Ecological Research Series
ENVIRONMENTAL TRACE MATERIALS
Computer Coupled Radioactivation Analysis
Environmental Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Corvallis, Oregon 97330
-------
RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into five series. These five broad
categories were established to facilitate further development and application of
environmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The five series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
This report has been assigned to the ECOLOGICAL RESEARCH series. This series
describes research on the effects of pollution on humans, plant and animal
species, and materials. Problems are assessed for their long- and short-term
influences. Investigations include formation, transport, and pathway studies to
determine the fate of pollutants and their effects. This work provides the technical
basis for setting standards to minimize undesirable changes in living organisms
in the aquatic, terrestrial, and atmospheric environments.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
-------
EPA-600/3-75-015
December 1975
ENVIRONMENTAL TRACE MATERIALS:
COMPUTER COUPLED RADIOACTIVATION ANALYSIS
by
Milton H. Feldman, David E. Cawlfield,
and Kenneth V. Byram
Laboratory Services Branch
Con/all is Environmental Research Laboratory
Corvallis, Oregon 97330
U.S. ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF RESEARCH AND DEVELOPMENT
CORVALLIS ENVIRONMENTAL RESEARCH LABORATORY
CORVALLIS, OREGON 97330
-------
DISCLAIMER
This report has been reviewed by the Corvallis Environmental
Research Laboratory, U.S. Environmental Protection Agency, and
approved for publication. Mention of trade names or commercial
products does not constitute endorsement or recommendation for
use.
ii
-------
CONTENTS
Section Page
I Conclusions 1
II Introduction 3
III Environmental Tracer Experiments 5
IV Experimental Procedure 7
V Environmental Monitoring By Radioactivation
Methodologies 19
VI Experimental Results 22
VII References 33
iii
-------
FIGURES
No, Page
1 Location of NB Buoy in New York Bight:
Experimental Sampling Site. 6
2 Equipment and Computer Connection. 11
3a Decay Plots, Sludge. 17
3b Decay Plots, Sediment. 18
4 Standard, Sludge, Sediment Spectra. 20
5 Standard, Sediment Spectra. 21
XV
-------
TABLES
No. Page
1 Irradiation, decay and counting time sequences. 8
2 Nuclide series considered. 9
3 Peak search printout. 14
4 Candidate nuclide printout. 15
5 Ranges of data from LSB and NAA. Run #1. 24
6 Comparison of some sludge data from LSB, NAA,
and NYSTP. 25
7 Sediments data showing candidate tracers. 29
8 Sediments data, replicates. 31
9 Cadmium content of phosphate ore and
fertilizers. 32
-------
ABSTRACT
A neutron activation laboratory with computer coupled equipment and
procedures was established. The power of the methodology for Environmental
Trace Material Analysis was demonstrated by analyzing various materials
and included quality control interlaboratory comparisons. Samples ranged
from sewage treatment plant sludges and marine sediments to fresh waters
containing very low concentrations of molybdenum, and ores and fertilizers
containing cadmium.
This report is submitted by the Corvallis Environmental Research
Laboratory, Corvallis, Oregon, under the sponsorship of the Environmental
Protection Agency.
VI
-------
SECTION I
CONCLUSIONS
FEASIBILITY OF RADIOACTIVATION ANALYSIS
Radiation methodologies for environmental trace materials research, in
particular neutron activation or the equivalent x-ray spectroscopic
methods, are feasible at laboratories with access to suitable irradiation
sources. Neutron activation analysis (NAA) is desirable for environmental
tracer experiments because it is sensitive and uses constitutent tracer
nuclides rather than introducing other tracers.
EQUIPMENT
Equipment designated as shelf items and fairly unsophisticated computer
programs are adequate for a good automated program of trace material
environmental research and monitoring; however, the cost may be signifi-
cant. The total cost of simple equipment described in this report was
about $40,000 (M972), plus access to a time sharing computer system and
a nuclear reactor. This estimate does not include the time and cost to
prepare and evaluate efficiency of computer programs.
COMPARISON AND REPLICATIONS
The comparison of analytical results indicates that either atomic
absorption (AA) or NAA can be used to analyze environmental trace
materials. However, the minimum size of samples that can be analyzed
differs greatly for the two methods. The use of higher flux (available
at numerous reactors) enables treatment of much smaller samples than
were handled in the development and routine work. Whereas, 100 mg
12
samples were adequate with ^ 10 , smaller samples can be assayed with
flux ^ 1014. In an investigation of molybdenum in lake waters, 10 ml
%
-------
14
water samples irradiated at a flux of £ 10 were shown to have molybdenum
_Q
content ranging from -0.68 to 0.81 x 10 gram/ml; typical AA procedures
can only detect 2.0 x 10~5 gram/ml using a 200 ml sample and resorting
to sample concentration techniques. Replication indicates adequate
precision to study changes, if they occur, on the order of 25 percent at
the microgram per gram level in 0.1 gram samples or, using higher flux
reactors, in 0.001 gram samples.
ENVIRONMENTAL SAMPLE ASSAY
Automated environmental monitoring with graphic display of "finger
prints" also may be carried out by NAA. For the sludge and sediment
samples considered in this work, gold, silver, and chromium are useful
elements for sludge tracing.
REFEREE METHODOLOGY
In addition to its general usefulness as a sensitive method for trace
analysis, NAA frequently is used as a referee or comparison method. For
example, phosphate ores and fertilizers were analyzed for heavy metal
content. The Environmental Protection Agency (EPA) laboratory in Region X
ascertained that some fertilizer and ores contained significant cadmium
and requested NAA for comparison. Results were obtained from radioactiva-
tion and compared with the results from AA using wet chemistry procedures.
As predicted by the observations of Bowen and Gibbons (1963), the results
were typically parallel, but NAA reported lower values.
-------
SECTION II
INTRODUCTION
STANDARD PROCEDURES FOR ENVIRONMENTAL TRACE MATERIALS
Although various chemical analyses of environmental samples have acquired
"standard procedure" status (Standard Methods, 1971) (Strickland, 1968)
(ASTM, 1972), the requirements for analytical chemical information grow
more stringent. Analysis of trace materials requires sensitivity and
precision adequate not only to discern the trace materials of interest
in surveillance sense, but also to enable following small changes in
their chemical, physical, and biological fates and mechanisms. Such
behavioral observations permit the computation (Morel, 1972) (Branica,
1968) and evaluation (Feldman, 1970) (Bowen, 1966) of the potential
ecological influence of trace materials.
The procedures utilized must be applicable to the specific matrix and be
amenable to some degree of routinization or automation since environmental
problems frequently involve numerous samples to define a field, or to
follow the behavior, and effect of a pollutant in the environment.
INTERCOMPARABILITY
Intercomparability of results of analyses from laboratory to laboratory
and studies of so called "standard samples" have not been utilized where
only environmental trends or changes have been studied; but such inter-
comparisons and standard sample analyses are now considered essential
(Feldman, 1964). (Bowen, 1964). It has been pointed out (Bowen,
1963) that historically the trace material analyst has tended
to report lower values for trace elements as chemical sophistication
advanced and that neutron activation analysis gives about as
-------
uncontaminated and direct a result as is presently available. It
should be recognized, too, that radioactivation procedures that utilize
nuclide characterization give not only a readout, but also positive
identification.
This is not only always the case where only a readout occurs as in atomic
absorption and atomic fluorescence spectroscopy. Problems and inter-
ferences, such as the severe iron interference in zinc estimations
(Kelly, 1973), or the sodium salt matrix interference with marine sample
trace element determinations by typical atomic absorption procedures,
require large blank corrections or prior chemical processing. But such
chemical processing is not feasible in the case of trace materials or
may lead to large, uncertain corrections dependent on numerous parameters
that require elaborate empirical handling (Brooks, 1967).
RADIOACTIVATION, A GENERAL METHOD
Radioactivation analysis provides a multielement, nondestructive capability
which meets the above provisos, for a fairly large group of elements
(Bowen and Gibbons, 1963). It does require elaborate experimental
facilities and is generally slower in output than atomic absorption. On
the whole, its susceptibility to automation and computer coupling is
better than most other procedures. Radioactivation does not measure
speciation since it measures the whole element independent of chemical
or physical form; it can distinguish between low concentrations whose
differences may result from speciation experiments (Strohal, 1973).
-------
SECTION III
ENVIRONMENTAL TRACER EXPERIMENT
APPLICATION OF RADIOACTIVATION
Radioactivation— specifically instrumental neutron activation analysis*
(INAA) based on Ge(Li) crystal detection with pulse height analysis and
computer coupled data handling and analysis—was used to estimate some
trace elements in sludges from sewage treatment plants in the New York
City area and in sediments from the New York Bight (Figure 1).
The principal objective of this work was to establish a trace materials
analytical laboratory capability for environmental research with procedures
based on computer coupled radioactivation, utilizing automated sample
handling and computer data analysis. As part of the procedural develop-
ment, analytical results were compared from the NAA laboratory at Corvallis,
a central laboratory service group (LSB) at Corvallis, and the New York
group (NYSTP) which operates the plants from which the sludge samples
were obtained.
A second objective of this work was to identify one or more suitable
constituent tracer nuclides in sludge that are not present at interfering
levels in the sediments. Then, after placing experimental quantities of
sludge on the ocean floor, it is feasible to follow the detailed movement
and chemistry, of the sludge materials when studied over a long period
of time.
I am greatly indebted to the Oregon State Board of Higher Education,
the Oregon State University, and Professor Chih Wang, Director of the
OSU Radiation Center, for permission to use the Radiation Laboratory
facilities with Program Director Status. MHF.
-------
40° N —
APPROXIMATE SITE
LOCATION
KILOMETERS
0 50
75°W
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SECTION IV
THE EXPERIMENTAL PROCEDURE
SAMPLE SIZE
Samples typically were about 100 mg for convenient handling, although
fractional mg samples can readily be analyzed at a slower pace and
higher cost.
WEIGHING
The introduction of automated weighing with electronic readout simplified
the laborious sample handling. Samples were placed in preweighed,
numbered vials of polyethylene, quartz, or aluminum (Battistone and
Feldman, 1966), then dried at 27°C. The weighings, on a Cahn Electro-
balance, were electronically read out and recorded in a notebook or
later were read out to a teletypewriter as well as indexed.
If circumstances require a preconcentration step (Joyner, 1967), (Feldman,
1967) (Rottschafer, 1971), or if the sample holder contributes trace
materials in instrumental neutron activation analysis (INAA), a small
blank may occasionally be necessary. It is generally the case that the
entire sample containing the component sought is encapsulated, irradiated,
and analyzed afterwards when interferences are minimized because the
element sought has been made distinguishable from the natural elements
present in the laboratory. The chief sources of contamination are from
the equipment used to procure the environmental sample and especially
from the laboratory dust itself.
-------
IRRADIATION
In order to identify potentially useful constituent trace nuclides, four
time groups of nuclides, irradiation and subsequent decay, and counting
were considered. The utility of this sequence has been demonstrated
(Dams, 1970) for air pollution studies. See Table 1 and Table 2.
(Hughes 1958, et seq).
TABLE 1. IRRADIATION, DECAY, AND COUNTING TIME SEQUENCES
'act Way
A 300 sec. 300 sec. 200-400 sec.
300 sec. 900 sec. 1000 sec.
B. 8-16 hr. 20-30 hr. 2000-4000 sec,
8-16 hr. 20 d. 4000 sec.
*
This period is easily adjusted after a preliminary examination
of the first sample of a set. The size of the adjustment, depends
on the number in the set and the half life group.
-------
TABLE 2. NUCLIDE SERIES CONSIDERED
O.I1 l.O1 101
Co 60m
Se 79m
Ag 108
Mn 56
Ni 65
Se 81m
Cu
Zn
As
Mo
Cd
Cd
Hg
Hg
64
69m
76
99
107
115
197
197m
TOO1 t?2r
Cr
Mn
Fe
Co
Zn
Se
Ag
Cd
Sb
Au
Hg
51
54
59
60
65
75
110m
115m
124
198
203
10.5m
3.9m
2.4m
2.6hr
2.56hr
57m
12.8hr
14hr
26.4hr
66.7
6.7hr
53hr
65hr
24hr
27d
31 Od
45d
5yr
243d
120d
255d
43d
60d
2.7d
47d
3
a
18
0.36
35
13
1.5
0.1
4.4
0.09
4.5
0.51
1
1.1
880
25
16
0.8(14)
1.1
19 + 18
0.5
30
3
0.14 + 1
3.3
100
4.0
%
100
23.5
51
100
1
49.8
69
18.6
100
23
1.2
28.9
0.15
0.15
4.4
100
0.31
100
49
0.87
49
.1 29
42.8
100
30
5
Y
58.5
95.9
619.0
846.7
1481.7
103.1
1345.8
439.1
559.1
739.7
93.0
527.9
77.6
133.9
320.1
834.8
1099.3
1173.2
1115.5
264.7
657.7
934.1
602.7
411.8
279.2
5
AI
2.4
12.2
1.8
100
24.7
98.8
0.48
100
44.6
13.7
4.8
27.5
20
34.2
9.8
100
56.5
100
52.4
59.5
94.4
2.5
98
96.8
81
6
1332.5
433.8
1811.2
1115.4
657.1
181.1
492.3
191.4
1291.5
1332.5
136.0
884.7
1289.9
6 7 7+8
AI v AI Y~%
0.
0.
29.
14.
6.
9.
8.
8.
43.
100
57.
75.
1.
025
54
4 2112.6 16
8 366.5 4.93
38
24 1216.3 3.4
5
1
9
5
35
2 279.5 24.6
1 937.5 34
03
1 - Group designated by half life region (hours)
2 - Precise half life
3 - Cross section, barns
11 - Abundance
5 - Principal gamma
6 - Second most prominent gamma
7 - Third gamma
8 - Annihilation
gamma as % of decays
-------
COUNTING
After suitable irradiation and decay a set of samples is placed in the
counting and recording system consisting of a Nuclear Chicago, Model
1035, mechanical sample changer, which is coupled in and controlled by a
Nuclear Data 2200 Pulse Height Analyzer (PHA). See Figure 2. The PHA
records signals (pulses from the 15% efficiency, 2.3% resolution, Ge(Li)
crystal*) in its 4096 channel memory through a 50 megaherz analog
digital converter (ADC). At the conclusion of a preset count period the
data are read out into either:
a. A telephone line feeding directly to the computer .
or b. A magnetic tape bulk data storage system based on Kennedy
tape transport model 3112.
Routine analysis utilizes the tape; experimental development work
utilizes either the wire or the tape or both. The tape is hand carried
to the computer at the end of a sequence of samples for subsequent
interrogation and printout of tables of data as allowed for in our
computer programs.
COMPUTER COUPLED NAA
The computer has proved very practical and helpful to handle large
quantities of data generated by the automated weighing, counting,
* 60
Compared to a 3" Nal crystal and using a Co 1.33 MeV line; by the
manufacturer, EDAX International, Prairie View, IL.
Oregon State University (OSU), Control Data Corporation 3300 + OSS
operating system.
10
-------
Nuclear Chicago 1035
Sample Changer
CAHN
ELECTRO-
BALANCE
Kennedy Tape
Transport 3112
OSU
Computer
CDC 3300 •+-
OS 3
Figure 2
-------
timing, accumulation and transmission of data from 4096 channels of the
PHA memory. Originally suggested as a desirable development a number of
years ago, (Fite, 1961), its development only became practical for
analytical chemistry with the advent of large Ge(Li) crystals. It
should be recognized that instrumental analysis alone sti11 cannot offer
all the criteria sometimes required by the analytical chemist, but this
is not to gainsay its great convenience. Many descriptions of detailed
and very ambitious programs* for computer coupled neutron activation
analysis have been published (Gunnik, 1972) for specialized usages where
sufficient numbers of chemical plant samples and work load justify the
specificity of program.
Our relatively unsophisticated programs which allow diversity of
application were each generated, as the need became obvious, as a
convenience to allow a technician to carry out simple laboratory procedures
and to have voluminous data handled for him as a substitute for rather
pedestrian data printing and hand computation. The program items presently
available allow for:
1. Area calculation of any "regions of interest" whose boundary channel
numbers are specified to the computer. These areas are corrected for
background, compared to standards similarly specified, and subjected to
standard deviation statistical examination. This program, particularly
useful for tracer experiments that generate many samples containing a
few known radionuclides, is also useful for computer interrogation that
experimentally evaluates a specific nuclide procedure for development.
*
Some such large detailed programs, carried out essentially in real time
and allowing for numerous samples and contingencies, effectively tie up
large computers. Unfortunately, even with fast front end and high speed
ADC, the data uptake rate and PHA is still a bottleneck.
12
-------
2. Calibration of the 4096 channels of the PHA for a range of energies.
This uses a set of standard materials (Dams, 1968) (Filby, 1970).
(Gunnik, 1969) or, more often, an element like europium-152 with several
well known gammas over the range of energies generally used. Comparison
of any unknown peak is by interpolation between the closest peaks used
in the calibration.
3. Peak searching by observation of changes of slope between successive
sets of channels by the procedure of Borchardt (1970), locates the edges
of the peak, the peak energy, estimates the area of the peak, corrects
for background, and estimates the standard deviation of the area.
Printout of this information comprises the essential data of our system
for quantification. See Table 3. Program item 4 which involves a
degree of judgment is of equal importance in developing reliable procedures
4. The computer program has access to a very complete library of data
on thermal neutron generated activities.* A printout of relevant data
on both sides of the energy of the peak of interest over any desired
energy span is easily evoked and printed out. Along with the gamma
energies there is printed out: nuclides, half lives, abundances, cross
sections, accompanying gammas. See Table 4. This information allows,
in most instances, decision as to identi y, as well as quantitation; in
some instances additional information from decay is required. Quittner
(1972) points out that energy and decay data generally are adequate for
positive identification as well as quantitation.
We are greatly indebted to R. H. Filby and his colleagues at Washington
State University for making available to us this valuable compilation of
data.
13
-------
TABLE 3. PEAK SEARCH PRINTOUT
Sediment A96M1B
UNKNOWN: J5T29
07/06/73 12:41 PM
No.
PCLa
Energy (keV)
Area
Error
Wgtc
Error
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
3 peak
b
33
169
178
185
192
239
262
268
287
315
351
381
392
413
429
486
526
556
621
637
678
685
502
822
963
991
1209
1218
1316
1530
1566
1592
1670
1771
1779
2096
2199
2242
2346
2581
2662
2688
2915
3092
3166
3296
3440
3636
1055
channel
19.7
87.3
91.8
95.3
98.7
122.1
133.5
136.5
145.9
159.9
177.7
192.6
198.1
208.5
216.5
244.8
264.7
279.7
312.1
320.1
340.5
344.0
352.5
412.3
482.0
495.8
604.6
609.1
658.2
765.0
782.9
795.9
834.8
885.2
889.2
1048.0
1099.6
1121.1
1173.2
1291.3
1332.0
1345.1
1459.1
1548.1
1585.3
1650.6
1723.0
1821.5
527.4
, . . .
15855
1719
1109
1955
4094
6355
7903
2298
8186
548
1338
3156
2056
1457
1409
729
1923
1080
7052
4709
726
4233
1092
7513
6411
1263
880
883
3023
895
168
575
1857
1135
15434
69
13521
14530
6456
9244
5998
26
1392
22
29
20
40
21
34
538
326
253
263
287
471
285
239
341
171
356
347
293
332
265
163
285
264
256
301
211
221
226
229
224
178
163
173
170
202
115
163
207
183
263
44
188
248
137
124
105
11
54
8
12
7
33
9
47
\
0
0
0
0
0
0
0
1.11
0
0
0
0
0
0
0
0
1.45
0
0
5.20
0
0
0
.31
0
0
0
0
2.65
0
0
0
0
1.75
0
0
0
0
2.28
0
2.41
0
0
0
0
0
0
0
7.92
0
0
0
0
0
0
0
.12
0
0
-
0
0
0
0
0
.22
0
0
.34
0
0
0
.01
0
0
0
0
.15
0
0
0
0
.28
0
0 ,
0 2.76° + .031
0
.05
0 2.34d + .031
.04
0
0
0
0
0
0
0
11.18
c weight of nuclide by comparison to a set of standards similarly counted
weight of nuclide by comparison to a separate standard by manual computation
14
-------
TABLE 4. CANDIDATE NUCLIDE PRINTOUT
Energy
Peak Energy =
335.8
336.0
336.2
336.6
337.3
338.3
339.9
340.0
340.5
341.6
Peak Energy =
843.8
844.3
844.7
844.9
845.4
845.8
846.5
846.7
848.9
Nuclide
338. 70a
51-SB-124
70-YB-169
49-IN-115M
31 -GA- 72
65-TB-160
32-GE- 77
61-PM-151
67-HO-166M
91-PA-233
71-LU-177M
846. 20a
12-MG- 27
32-GE- 77
46-PD-111M
52-TE-129M
63-EU-154
36-KR- 87
54-XE-125
25-MN- 56
61-PM-151
Half -Life
6.03E+01D
3.18E+01D
4.50E+OOH
1.41E+01H
7.21E+01D
1.13E+01H
2.78E+01H
1.20E+03Y
2.70E+01D
1.61E+02D
9.46E+OOM
1.13E+01H
5.50E+OOH
3.41E+01D
1.60E+01Y
7.60E+01M
1.68E+01H
1.55E+02M
2.78E+01H
X-Sect
3.30E+00
1.10E+04
5.00E+00
4.60E+01
l.OOE+01
l.OOE+00
l.OOE+00
2.70E-02
l.OOE-01
4.00E-02
1.70E-02
3.20E+02
6.00E-02
1 .10E+02
1.33E+01
ABUN
42.75
.14
39.80
99.99
7.67
99.99
2.60
11.29
7.67
11.81
31.79
52.23
17.37
.10
99.99
Association
Gammas
603
64
834
879
264
168
185
312
208
1015
264
172
696
123
403
188
1811
340
1691
197
2202
299
211
275
811
300
229
171
211
70
730
1274
2556
243
2112
168
a Where the observed peak energy 338.70 was entered, the computer printed
the data on known species in that vicinity i.e., energy, nuclide, half life,
cross section, abundance of isotope and associated gammas.
15
-------
Decay information of a given peak or set of peaks in a sequence of
counts is always desirable in developing procedures for samples of a
newly given set. The use of the tape for recording a set of samples'
changing spectra with time by repetitive counting in the mechanical
sample changer gives a set of data that can easily be used for this
purpose. Thus, suppose 18 samples are counted ten times in a 48 hour
period. Then the tape data in the computer are queried for a given peak
(region of interest per program item 1) in repetitive spectra for a
given sample or samples and the results plotted using a simple least
squares statistical evaluation to obtain the decay constant for each
nuclide peak of interest.
See Figure 3a, 3b. The intercept, at time 0 is used for quantitative
comparisons, while the positive identification is obtained from the
combination of the t, ,2 °f program item 5, with the E obtained in
program item 3 and the candidate nuclide information printout of program
item 4.
16
-------
1000-
14 APRIL 1973
100-
= 4I2
= 66hrs.
1
^
Q:
E= 1368
E=559
f'/2 = 15 hrs.
= 26 hrs.
E = 657
V
0
24
48
HOURS
17
72
96
Figure 3 a
-------
Sediment D96 M4
o
<
0>
>
-------
SECTION V
ENVIRONMENTAL MONITORING BY RADIOACTIVATION METHODOLOGIES
"Finger printing" and detection of very small changes in environmental
samples is an important spinoff of neutron activation procedures easily
presented by analog (graphic) display of the data. While not quantita-
tive, as are the procedures described above, it does allow quick display
of spectroscopic "finger prints." Generally such a display offers more
information than can be readily grasped by eye and understood. However,
the analog display considered as a picture can be very useful in a
monitoring sense since changes or differences can be noted and later
determined precisely by recall from the tape storage system and computer
interrogation.
For example, planning sessions to evaluate a proposed experimental site
raised the question: Since the size of sediment particles changes from
point A to point B, accompanied by apparent changes in benthos are the
two changes related or is this caused by a chemical change? Graphic
display (see typical sediment spectra in Figures 4 and 5) allowed prompt
application of chemical information to this question. The two actual
spectra showed no obvious chemical difference, so biological differences
seemed more likely to be related to particle size differences.
19
-------
COMPOSITE STANDARD
v Au
V i
. 320 . . 603
279 412 564 §57
. 1115
1099
SEDIMENT *AI02-M3
-------
CALIBRATION EU
152
121.8
344.:
SEDIMENT No. D96M4
COMPOSITE Au
STANDARD
As As
I Cd Asl
52,7.9] 657,1
411.8 559 675
1368
Figure 5
-------
SECTION VI
EXPERIMENTAL RESULTS
SAMPLES
Samples for analysis included sewage treatment plant sludges from
various New York City area plants* and sections of 4" cores from the N.
B. Buoy area (lat. 40°24'N, Ion. 73°11'W) about 15 miles south of the
Fire Inlet on the south shore of Long Island. See Figure 1.
In Con/all is the Laboratory Services Branch (LSB) used AA and the NAA
laboratory used INAA to analyze the sludge samples. A parallel set of
monthly composite sludge samples, by the New York area sewage treatment
plant operators (NYSTP) used AA to analyse.
Thus, while the sampling, storage, transport, and analytical approach
and actual nuclides measured are not identical for all three analytical
groups there is enough overlap to make valid comparisons.
The sampling procedures of all three groups are considered reliable and,
in view of the substrate's variable nature, quite adequate for these
analytical purposes. Because LSB and NYSTP analyzed "wet samples" and
dried a parallel sample to get dry weight equivalence, their numerical
results have been made comparable with information from the total solids
determinations.
*
Obtained through the cooperation of Richard Dewling, Al Bromberg, and
Dr. Richard Spear of EPA, Region II,
Obtained for us by various members of our staff, Dr. R. Swartz, A.
Teeter, W. DeBen.
22
-------
RANGES OF VALUES NAA/LSB
Table 5 compares some early NAA results with LSB results from well
practiced AA procedures to show the range of values from eight sludge
samples analyzed for various nuclides. No comparison is made when
either LSB or NAA did not assay that nuclide. Evidently the two methods
produce reasonably comparable results for aliquots taken from the same
samples.
DETAILED ANALYSES—NAA, LSB, NYSTP
Table 6 compares a larger set of detailed data from NAA, LSB, AND NYSTP
analyses. Since NAA and LSB used closely related samples, their results
compared more closely than the NYSTP results. The NYSTP group analyzed
a monthly composite; consequently its single result is tabulated against
several NAA and LSB results from several samples variously collected
during that given month.
SEDIMENTS
Table 7 shows sediment results analyzed by NAA alone. Remembering that
the lower intensity peaks could be analyzed, the primary purpose here is
to establish that gold, chromium and silver, if present, are low, and
may be used as tracers within the sludge. Therefore, a— or (blank)
only means that the nuclide activity is low or has not been estimated.
Table 8 shows the results from four sections of a core, each section
divided into three equivalent samples and subjected to increasing amounts
of washing and, incidentally, to increased amounts of handling. Replica-
tion shown in this table indicates that changes on the order of 25% at
the microgram per gram level in 0.1 gm samples, or using high flux
levels with 0.001 gm samples, could be studied.
23
-------
TABLE 5. RANGE OF TRACE ELEMENT CONCENTRATIONS IN SLUDGE
(eight samples from N.Y. area)
Cd
Cr
Co
Cu
Fe
Pb
Mn
Hg
Ag
Au
As
Se
LSB
10-400
200-800
7-20
800-1800
~104
17-860
240-560
10-20
NAA
(ppm dry weight)
400-1800
15-36
550-900
HO3]9
200
[ 21-37]b
6-13
2-4
5-1 3C
0.5-1
a Calc on Ag standard in absence of Fe Standard
Calc on Cr standard in absence of Hg standard
c Average As was 9 ppm; extremes 5, 13 in eight sludges
24
-------
Table 6a
SLUDGE INTERCOMPARISON
Sample
NAA 33501
LSB
NYSTP
NAA 33502
LSB
NYSTP
NAA 33503
LSB
NYSTP
NAA 33504
LSB
NYSTP
NAA 33505
LSB
NYSTP
NAA 33506
LSB
NYSTP
NAA 33507
LSB
NYSTP
NAA 33508
LSB
NYSTP
Location
Tall man
Island
Tallman
Island
Jamaica
Bay
Tallman
Island
Jamaica
Island
Tall man
Island
Jamaica
Island
Tallman
Island
Se
Date (136)
6 July 72 0.54±.26
July Ave.
11 July 72 0.95±.35
(ave)
11 July 72 0.92+.25
(ave)
23 July 72 0.66±.21
(ave)
21 July 72
(ave)
28 July 72 0.46+.18
(ave)
28 July 72 0.72±.20
(ave)
4 Aug. 72 0.67±.25
(ave)
Hg*
(279)
22
8
15
26
9
15
28
11
72
21
12
15
9
72
28
8
15
36
5
72
26
12
15
.3
.9
.0
.9
.4
.0
.9
.0
.0
.2
.0
.0
.2
.0
.9
.3
.7
.9
.0
.1
.0
.0
Cr
(320)
964± 71
780
910
1413±104
820
910
586± 44
350
460
1050± 78
765
910
300
460
428± 33
980
910
562 ±42
325
460
1762±130
980
1270
Au Ag
Co
(412) (658) (1173)
2.18±.19 10.6±.2 22.
15.
3.76 .44 13. 5± .3 35.
17.
1.9U.24 8.48±.3 14
14
2.06±.26 10.5+.2 26
16
2.85±.49
11
3.94±.28 5.5U.2 24
16
3.07±.18 6. 90+. 2 19
11
4.34±.45 12.8±.3 31
7
7± .8
5
7±1.1
0
.3±.67
.0
.7±1.0
.0
.0
.5± .95
.0
.7± .72
.0
.9+1.1
.0
Fe
mg/g
(1099)
20.
20.
5
0
20.0
20
22
19
20
20
22
20
20
20
19
18
26
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
.0
Mn
(847)
259±2.
240
242+2.
240
350 ±2.
560
215+1.
275
415 ±2.
430
570 ±3
240
258 ±1
430
189 ±1
225
3
2
0
5
.7
.1
.8
.6
Calculated from standard Cr in absence of Hg standard
**Numbers in parentheses under nuclide are approximate
energy of gamma observed in keV
All results in ppm dry weight basis except Fe
-------
Table 6b
SLUDGE INTERCOMPARISON
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
Sample
39501
39502
35903
39504
39505
39506
39507
39508
39509
39510
Location
Tall man
Island
Jamaica
Bay
Tall man
Island
Jamaica
Bay
Tall man
Island
Jamaica
Bay
Tall man
Island
Jamaica
Island
Tall man
Island
Jamaica
Bay
Date
11 Aug. 72
(ave)
11 Aug. 72
25 Aug. 72
25 Aug. 72
1 Sept- 72
1 Sept. 72
13 Sept. 72
13 Sept. 72
14 Sept. 72
14 Sept. 72
Se
(136)
5.17+1.5
3.8&+1.5
5.89±1.5
5.51+1.7
9.02+2.4
4.70+1.3
5.04 1.8
4.0U1.6
5.34±1.7
2.92 1.3
Hg
(279)
11.6+1.2
55.0
10. 3± .85
55
10. 0± .94
55.0
10.7+1.10
46.0
11.7+1.3
18
44
11. 9± .97
10.0
116
11.1 ±1.4
11.0
44
11.1+1.2
5.0
116
8.39+ .81
7.9
44.0
10. 3± .91
116
Cr
(320)
290
1272
7C4+22
550
714+23
1272
325 ±11
550
757+24
1200
818
363+12
476
1180
755+24
1200
818
368+12
500
1180
755 ±25
1100
818
363+12
410
1180
Au Ag
(412) (658)
7.29±.06 30.8+2.5
4.62+.05 56.9+43
5.96±.05 58.7+ 4.4
4.53+.05 30.6+ 2.4
5.79+.06 72.5+ 5.6
6.11±.04 32.2+2.5
8.59+.07 57.4±53
10. 1± .07 26.5+2.6
5. 80+. 05 56.3±5.2
4.21±.04 29.1±2.7
Co
(1173)
2.99±.09
1.94+.08
2. 27+. 08
2. 49 +.10
3.35+.12
7.5
2.38+.08
10.0
3.22+.11
8.1
2.78+ .09
6.5
2.67+ .09
6.8
2.40+ .08
11.0
Fe mg/g
(1099)
26.0
28.0
26.0
28.0
17.0
11.0
16.0
21.0
16.0
11.0
15.0
21.0
12.0
11.0
14.0
21.0
Mn
(847)
449 ±5
278±4
310+2
473±3
288±2
280
447+2
476
343±3
343
464±3
395
273±2
272
-------
Table 6c
SLUDGE INTERCOMPARISON
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
Sample
42501
42502
42504
47501
47502
47504
Location Date
Tall man
Island 21 Sept. 72
Jamaica
Bay 21 Sept. 72
Jamaica
Bay 28 Sept. 72
Tall man
Island 6 Oct. 72
Jamaica
Bay 6 Oct. 72
Jamaica
Bay 13 Oct. 72
Se
(136)
3.08+1.2
6.07±2.4
1.34± .94
3.56±1.0
3.3U1.1
3.90±1.3
Hg
(280)
8.75± .89
18.0
44.0
11.4±1.2
12.0
116.0
10.4±1.2
9.2
116.0
8.45+.61
21.0
57.0
7.48±.75
35.0
42.0
8. 59+. 68
19.0
42.0
Cr
(320)
667±21
100.0
818
417±14
62
1180
288427
93
1485
612±27
93
1485
244 ±10
44
540
283±13
50
540
Au
(412)
5.8±.07
3.81±.05
4.17±.06
4.58+.05
3. 81 ±.07
6.19±.05
Ag
(658)
49.1±5.
32.9±3.
73. 8± .
58. 1± .
96. 6±.
99. 6± .
Co
(1173)
1 254±.08
7.9
2 1.34±.15-
12.0
10 2.45±.09
9.4
08 2.39±.07
10.0
07 1.74±.07
9.1
09 2.46±.08
7.7
Fe
(mg/g)
(1099)
17.0
10.9
16.0
21.0
19.0
21.0
15.0
28.0
15.0
26.0
16.0
26.0
-------
Table 6d
SLUDGE INTERCOMPARISON
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
NAA
LSB
NYSTP
Sample
45801
48502
52501
52502
52503
52504
52505
52506
52507
52508
52509
Location
Rockaway
Island
Coney
Island
Coney
Rockaway
Coney
Rockaway
Coney
Rockaway
Coney
Rockaway
Coney
Se Hg
Date (136) (280)
8 Nov. 72 4.49±2.2
31.0
275
8 Nov. 72 2.89+1 .9
20.4
35.0
14 Nov. 72 4.44±1.9
17.
35
24 Nov. 72 3.56+ .10
9.3
27.5
24 Nov. 72 4.14+1.9
10.7
35.0
29 Nov. 72
6.3
275
29 Nov. 72 4.29±2.9
12.5
35
6 Dec. 72
8.8
32
6 Dec. 72 7.73±2.5
18.5
28.0
13 Dec. 72
9.3
32
13 Dec. 72 3.35±1.4
12.7
28
Cr
(320)
202 ±1 5
285
222
346+22
327
242
355±22
442
242
107+7.1
112
222
236±15
291
242
34±5.6
38
222
297±15
341
242
59.9±5.2
70
68
29H15
336
182
31.6±3.7
100
68
294±12
327
182
Au Ag Co
(412) (658) (1173)
1.79±.08 83.5i3.4 5.24±.46
2.33±.05 71 .2+3.1 6.71 ± .44
2.43±.04 74.U4.0 6.74±.50
0.93± .03 30.4±1.7 5.04±.32
4.44± .07 53.5±2.4 5.59±.41
0.25± .03 10.6±1.4 2.27±.39
2.74± .09 66.6±4.7 7.54±.80
0.58± .06 22.8±1.9 0.50±.26
2.98± .07 68.3±3.9 6. 35+. 65
0.22± .05 10.9±1.5 3.91±.49
74.4±3.7 5.61±.41
Fe (mg/g)
(1099)
18. 1± .4
21
10
18. 0± .4
16.3
14.0
17.6±.4
17.7
14.0
17.3
17.0
10.0
14.3±.3
14.2
14.0
4.99+3
6.0
10.0
19.8+ .5
19.1
14
7.03+.3
8"
12
17.9+ .5
18.7
14
4.40+.3
4
12
17.8+ .4
17.8
14
-------
TABLE 7a
Sediment Core Section Analyses
Core
Location Cut
E99
A90
B86
C89
D96
D99
Ml
M2
M3
Ml
M2
M3
M4
Ml
M2
M3
M4
Ml
M2
M3
M4
Ml
M2
M3
Ml
M2
M3
M4
Date (136)
2/21/73 8±.5
U.6
U.6
1±.5
1±.6
2±1
U.6
2±1
1±.7
2±.7
U.5
U.5
1±.7
U.7
1±.7
Se
(264J
8±.7
.4±.4
U.6
.5±.3
.U.3
U.8
.U.3
U.7
.4±.5
U.5
.U.3
U.7
U.7
U.8
Cr
(320)
4±1
3+1
5±1
3±1
5±2
4±2
2±1
5+1
3±1
3±1
4±1
3±1
4+1
6±1
8±2
9±2
8±2
9±2
2±1
4±1
2 i
Au Ag
(412) (657) (764) (937)
5±3
.03+. 01 2±1
.9±.4 1±1
U.5
.03+. 01 .9+. 5 2±1 Ul
.02+. 01
.7+. 5 2±1
U.4
.8±.3
3±.5 3±2 2±1
U.4
U.7 2±1
2±1
.5±.3 2±1 .2 + . 4
2±1
.03±.01
.02 iOl
Co
(1172) (_133_2_)_
1±
.4±
1±
.6 +
.7±
.2 +
.6 +
.6 +
]±
]±
.1
.1 .6+.1
.1
.1
.2
.1
.2
.1
.2
.2
.4+.1
.7+
.2 +
.8+
.2 +
U
U
.U
U
J±
.4+
.U
.6
.1 U.I
.1 U.I
.1
.1
.2
.2
.2
.2
.1
.1 .6 + .1
.1
+1
Fe (mg/gm)
(1009)
4±.2
5±.l
U.I
2+.2
U.I
U.I
U.I
U.I
8±.2
8+.2
7±.2
7+.2
2±.l
2±.l
2+.1
2 +1
(1291)
4±.2
4+.2
U.I
U.I
U.I
8±.2
8±.3
7±.2
7±.2
2±.l
2 +1
Sc
(899)
8169
4474
7850
3852
1983
1959
2003
1600
9519
1628
1655
6997
4509
5485
3415
5594
4361
4131
5643
2802
4508
3820
4489
(1120)
6422
3950
7065
2413
1708
1581
1760
1452
8023
1706
1574
5652
4082
4107
2807
4831
3389
3389
4317
2496
4608
3583
3716
All results ppm dry weight basis except Fe (mg/gm) and Sc results are relative counts only
-------
TABLE 7b
Sediment Core Section Analyses
Location
F102
G
H
J99
199
Core
Cut
Ml
M2
M3
M4
Ml
M2
M3
M4
Ml
M2
M3
M4
Ml
M2
M3
M4
Date (136)
22/2/73
1 + .7
1+.8
2+1
1 + .4
3+.6
3+.7
3+.9
1+.5
Se
(264)
2+1
.5±.4
1 + .4
.3 + . 3
2±.7
1+.6
1 + .7
1±1
1±.5
1±.8
1±.6
Cr Au Aq
13201 (412) (657) (764) (937)
3±1 .05±.03 5+3
3±1
5±1
2±1
3+1
4±1 .09±.03 .3±2
3±1 .04+. 02
2±1
10±2 7+2
14±2
12±2 1±.5 .6+1
16±2 1±.6
3±1 2+1
3±1
3±1 1 + .3
2 + 1 ]±.5 1±.7
(11
1±
1±
1±
1±
.5±
.1 +
2+
2±
2±
1 +
.7±
.3±
.5 +
.5±
Co
73) (1332)
.2
.2
.2
.2 l+.l
.1 l + .l
.1
.1 l + .l
.2 l + .l
.2 2+.1
.2
.2
.1
.1
.2
.1
Fe (mg/i
(1009)
2+.1
2±.2
3±.2
2±.2
2±.l
2±.l
2±.l
3±.l
3±.l
3+.1
5±.2
l+.l
l±.l
i+!i
gm)
(1291)
2±.
3±.
3±.
2+.
2±.
3±.
3±.
3±.
4+.
^-
1
2
2
2
1
1
1
1
2
(899]
4312
3267
2929
2607
2680
2607
3558
2885
26,629
29,807
23,408
22,313
1570
1187
1580
2781
Sc
1 (1120)
4000
2820
2200
1988
2515
1938
2453
2303
21,428
24,954
17,300
17,678
1480
1168
2663
All results ppm dry weight basis except FE (mg/gm) and Sc results are relative counts only
-------
Sample Date
A 96 Ml A* 21 May 73
A 96 Ml B
A 96 Ml C
A 96 M2 A
A 96 M2 B
A 96 M2 C
A 96 M3 A
A 96 M3 B
A 96 M3 C
A 96 M4 A
A 96 M4 B
A 96 M4 C 21 May 73
*Each sample, e.g.
Replicate
1
2
3
1
2
3
1
2
3
1
2
3
A-location
96-depth of
Ml • M2' M3*
Lab
Number
268
272
276
280
284
288
292
296
300
304
308
312
on Grid
water in
M. -si ice
Se
036)
1.13± .13
1.11± .12
1.33± .12
1.89± .18
2.21± .20
1.72± .13
3.29±1.6
1.86± .14
2.13± .16
1.69± .13
ft.
of core
(264)
1.6U.15
1.45±.22
1.311.16
1.43±.14
1.391.15
2.091.19
2.07±.35
2.02±.17
1.98±.21
2.06±.25
1.36±.16
1.35±.18
was
A,
Table 8
Cr Au
(320) (411)
5.77±.28 0.32±.01
5.20±.34 0.31±.01
5.24±.33 0.27±.01
7.001.43 0.34±.01
5.28±.25 0.37±.01
7.77±.49 0.50±.01
8.02±.30 0.451.02
7.00±.44 0.45±.01
7.87±.42 0.38±.02
6.97±.32 0.43±.01
7.55±.38 0.36±.01
6.07±.23 0.3U.02
divided into 3 aliquots
B, C for analysis as
Ag
(658)
2. 66+. 24
2.65±.15
2.62±.22
3.40±.22
3.89±.21
3.95±.22
4.06±.28
4.12±.28
3.41±.23
3.79±.24
2.92±.19
2.91±.25
(885)
0.7U.29
1.75±.28
2.3H.26
1.451.37
0.701.35
1.721.32
0.531.31
1.321.36
0. 96+. 27
0. 04+. 31
Co
(1173)
2.101.05
2.281.05
2.101.04
2.411.06
2.601.05
3.28+.06
3.15+.07
2.791.06
2.65±.05
2.841.06
2.231.04
2.231.05
(1332)
2.451.04
2.4U.04
2.231.04
2.691.04
2.65+.04
3.381.05
3.211.05
2.911.05
2.901.05
2.991.04
2.451.04
2.421.04
Fe (mg/gm)
(1090)
2. 52+. 04
2.261.03
2.37+.03
2.891.04
2.841.04
2.991.03
3.301.04
2.841.03
3.391.03
3.241.03
3.961.04
4.341.04
(1291)
2.601.03
2.341.03
2.401.03
2.90+.03
2.851.03
3.101.04
3.4U.04
2.891.03
3.3U.03
3.321.09
3.8U.03
3.111.03
separate samples.
-------
Table 9 shows a comparison of results from radioactivation of ores and
fertilizers with the results from AA and wet chemistry. The two different
methods of analysis, A.A. and NAA, at two different laboratories give
parallel results. Their ratio was AA/INAA = 1.72 + .34.
TABLE 9. CADMIUM CONTENT OF PHOSPHATE ORE AND FERTILIZER
Lab #
33802
38803
38804
38807
38808
38812
38813
38815
38820
38821
38822
38826
Sample
f erti 1 i zer
fertilizer
f erti 1 i zer
fertilizer
f erti 1 i zer
f erti 1 i zer
fertilizer
fertilizer
fertilizer
fertilizer
Ore
Ore
Vial
1
2
3
4
5
6
7
8
9
10
11
12
NAAa
24
49;48b;47b
34
50
45
59;68b
111
16
102
76
90
AA
42
86
80
108
84
50
114
154
20
140
106
161
results are yg Cd per gram sample, dry weight.
same standard but counted at a later time.
32
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SECTION VII
REFERENCES
ASTM 1972. Annual Book of ASTM Standards, 1972. Part 23 Water: Atmos-
pheric Analysis. American Society for Testing Materials, Philadelphia,
PA.
Battistone, G. C. and M. H. Feldman. 1966. Sample Handling Conveniences
for Activation Analysis. Int. J. Appl. Rad. Isotopes. 17:74-75.
Borchardt, Glenn A., Gordon W. Hoagland, and Roman H. Schmitt. 1970.
Spectra, A Computer Program for the Analysis of Gamma Ray Spectra.
J. Radioanalytical Chemistry 6;241.
Bowen, H. J. M. and D. Gibbons. 1963. Radioactivation Analysis. Oxford
Press. (Table 10.4 on p. 160 shows recent activation vs. older wet
chemistry results.)
Bowen, H. J. M. 1964. Int. Conf. on Activation Analysis (NATO) in
Glasgow, Scotland. Dried Kale Leaves as Possible "Standard Material"
for Neutron Activation Analysis.
Bowen, H. J. M. 1966. Trace Elements in Biochemistry. Academic Press,
London.
Branica, M., M. Petek, A. Baric and L. J. Jeftic. 1968. Polarographic
Characterization of Some Trace Elements in Sea Water. Proc. XXX
C.I.E.S.M. Congress, Buchaarest. 1966 Rapp Uomm Int. Mer Medit. 1_9:102-
106.
Brooks, R. R., B. J. Presley and I. R. Kaplan. 1967. APDC-MBIK Extrac-
tion System for Determination of Trace Elements in Saline Waters by
Atomic-Absorption Spectrophotometry. Talanta 14: 809-816.
Dams, R. and F- Adams. 1968. Gamma Ray Energies of Radionuclides
Formed by Neutron Capture Determined by Ge(Li) Spectrometer.
Radiochimica Acta. 10:1.
Dams, R., J. A. Robbins, K. A. Rahn, and J. W. Winchester. 1970. Non-
destructive Neutron Activation of Air Pollution Particles. Anal.
Chem. 42(8):861.
33
-------
Feldman, M. H., R. C. Reba and 6. C. Battistone. 1964. Presented at
Int. Conf. on Activation Analysis (NATO) in Glasgow, Scotland.
Simplified Rapid Determination of Manganese in Biological Specimens
by Neutron Activation Analysis.
Feldman, M. H., J. McNamara, R. C. Reba, and William Webster. 1967.
Protein-Bound Iodine, Determination by Activation Analysis. J.
Nucl. Med. 8_:122-130.
Feldman, M. H. 1970. Trace materials in Waste Disposed to Coastal
Waters: Ecological Guidance and Control. Working Paper #78. Fed.
Wtr. Pollution Control Admin., Pacific Northwest Water Laboratory,
Corvallis, Oregon.
Filby, R. H., A. I. Davis, K. R. Shah, G. G. Wainscott, W. A. Mailer,
and W. A. Cassatt. 1970. Gamma Ray Energy Tables for Activation
Analysis. Pub. #97(2), Washington State University,
Fite, L. E., D. Gibbons, and R. E. Wainerdi. 1961. Computer Coupled
Activation Analysis. TEES 2671-1 UC-73 Texas Eng. Exp. Station,
College Station Texas.
Gunnik, R., and J. B. Niday. 1972. Computerized Quantitative Analysis
by Gamma-Ray Spectrometry, I The Gamanal Program. Lawrence Livermore
Laboratory. Pub. No. UCRL-51061
Gunnik, R., J. B. Niday, R. P. Anderson and R. H. Meyer. 1969. UCID
15439. Gamma Ray Energies and Intensities.
Hughes, D. J. 1958. Neutron Cross Section Charts and Nuclear Data.
Brookhaven National Laboratory, Publication No. 325.
Hughes, D. J. 1960. Neutron Cross Section Charts and Nuclear Data
Supplement 1. Brookhaven National Laboratory. Publication No.
325. One volume.
Hughes, D. J., 1966. Neutron Cross Section Charts and Nuclear Data,
Supplement 2. Brookhaven National Laboratory. Publication No,
325. Three volumes.
Joyner, T., M. L. Healy, Diptinian Chakravarti, Taku Koyanagi. 1967.
Preconcentration for Trace Analysis of Sea Waters. Env. Science
and Technology. 1_(5):417.
34
-------
Kelly, W. R., and C. B. Moore. 1973. Iron Spectral Interference in
Determination of Zinc by Atomic Absorption Spectrometry. Anal.
Chem. 45(7):1274.
Morel, Francois and J. J. Morgan. 1972. A Numerical Method for Computing
Equilibrium in Aqueous Chemical Systems. Envir. Science and Tech-
nology 6_(1):58.
Quittner, P. 1972. Gamma Ray Spectroscopy. Adam Hilger Ltd., London.
Rottschafer, J. Mark R. J. Boczkowski, and H. B. Mark, Jr. 1971. Pre-
concentration Techniques for Trace Analysis via Neutron Activation
Talanta 1_9:63.
Standard Methods for the Examination of Water and Waste Water. 13th ed.
Am. Pub. Health Assoc. Washington, D.C. 1971.
Strickland, J. D. H. and T. R. Parsons. 1968. A Practical Handbook of
Seawater Analysis. Fisheries Res. Board Bull. 167. Queens Printer,
Ottawa, Canada.
Strohal, P. and T. Pinter. 1973. Thorium in Water and Algae from the
Adriatic Sea. Limnol. and Oceanography. 18(2):250.
35
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-600/3-75-015
3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
5. REPORT DATE
ENVIRONMENTAL TRACE MATERIALS: COMPUTER COUPLED
RADIOACTIVATION ANALYSIS
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Milton H. Feldman, David E Cawlfield,
Kenneth V. Byram
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
U'. R. Environmental Protection Agency
Corvallis Environmental Research Laboratory
200 S.W. 35th Street
Corvallis, Oregon 97330
10. PROGRAM ELEMENT NO.
1BA025
11. CONTRACT/GRANT NO.
12. SPONSORING AGENCY NAME AND ADDRESS
13. TYPE OF REPORT AND PERIOD COVERED
Final
same as above
14. SPONSORING AGENCY CODE
EPA-ORD
15. SUPPLEMENTARY NOTES
16. ABSTRACT
A neutron activation laboratory with computer coupled equipment and procedures
was established. The power of the methodology for Environmental Trace Material
Analysis was demonstrated by analyzing various materials and included quality
control interlaboratory comparisons. Samples ranged from sewage treatment plant
sludges and marine sediments to fresh waters containing very low concentrations
of molybdenum, and ores and fertilizers containing cadmium.
This report is submitted by the Corvallis Environmental Research Laboratory,
Corvallis, Oregon, under the sponsorship of the Environmental Protection Agency.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Group
3. DISTRIBUTION STATEMEN1
19. SECURITY CLASS (This Report)'
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