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MICROCOPY RESOLUTION TEST CHART
NATIONAL BUREAU OF STANDARDS -1963
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MASTER

3:967
JUN
II. ANALYSIS OF SOLUTI ON AND RADI OACTIVE SAMPLES
BY SPARK SOURCE ASS SPECTROMETRY*
CFSTI PRICES
J. A. Carter
-
no. 300 mn.,6.5
The first radioactive materials analyzed in the MS-7 at ORNL were a
series of chromium-technetium alloys ior trace impurities as well as the
Tc concentration. The impurity results were evaluated by the visual
technique while the Tc results were evaluated by plotting the exposure vs
percent transmittance and using the standard boron calibration curve as
in Siire :
SLI DE I
with the necessary mathematical corrections to convert to wt % Tc. 'Ic and
B have ussentially the same spark sensitivities as can be seen from the
comparative results in Slije II.
SLI DE II
We have analyzed uranium metal and uranium as the oxide, sulfide, phosphide
and nitride. The uranium compounds were mixed with high purity Ag a70
pressed in an isostatic press. After a suitable set of exposures are made,
the photoplates are evaluated by the visual method. In general the
elements of most interest are those with high neutron cross sections.
A tungsten-rhenium thermocouple wire that had been irradiated was
recently run for Os and Ir. The sample had an activity of 10 mr/hr. The
analysis showed 1100 ppm Os and 6 ppm Ir. After this analysis, the source
was disassembled and the radioactivity of the various parts measured. All
of the items are standard AH components as shown in Table I. with the
corresponding activity distribution.
TABLE I
The majority of radioactivity was found on the first slit. Since this
slit can easily be removed and cleanec, or even discarded, we expect to be
able to run low to medium le, radioactive samples without a great deal
of difficulty.
*Research sponsored by the U. S. Atomic Energy Commission under contract
with the Union Carbide Corp.
DISTRIBUTION OF THIS DOCUMENTI 19. UNLIMITEL
-2-
In the analysis of more highly radioactive sampies, the amount of
sample is limiced from a health and radiation stand point. We have found
that to facilitate the handling of small sample aliquotes, it is best to
dissolve the sample. This in some cases nay introduce some impurities,
but the improved handling ease greatly outweighs this disadvantage.
Also, the solution enables one to add an internal standard and to improve
the homogeneity of the bulk sample. A minor difficulty is that one must
interpret the data fro the same exposure as the internal standard is
measured; therefore, it is important to pick an internal standard with a
range in isotopic abundance. Two internal standards that we have used
are In and Sr.
The data shown in Slide JII are some of the early results obtained on
several solutions. The total sample size was approximately 10 micrograms.
SLI DE III
in the analyses a droplet of solution was put onto each rod and evaporated.
There was no electrostatic field to hold the droplets. The electrode rods
were approximately 1/8" in diameter with a metal center post 1/16" x 1/16".
The electroes were sparked end to end.
Another example of the type of qualitative to semiquantitative results
obtained are the normalized results presented in Table II
TABLE II
of some irradiated corrosion products. Because of the radioactivity these
samples were solutioned in hot cells and approximately 5 ug of material
added to the electrodes from the analysis.
We are preparing for the analysis of Pa. In this study, we will
only be able to handle in our cold lab no more than 2 micrograms of sample
and we want to know the impurities present at about the 0.5% level.
Table III shows the results for the analysis of Nb in U. These samples were
prepared and analyzed exactly as we will handle the 23 Pa sample.
TABLE III
All of the results wer road from a single exposure using In as the internal
LEGAL NOTICE
standard.
This report was prepared u an account of Government sponsored work. Matthar the United
States, por the Cominjasivn, nor any person acting on behalf of the Comalesioa:
A. Makes any warranty or representation, expressed or implied, with respect to the accu-
racy, completoneau, or usefulness of the information contained in the report, or that there we
of way information, apparatua, method, or procou discloned in the report may not infringo
privately owned rights; or
B. Asamos nay Habilities with respect to the war of, or for duper rent from the
use of any inforastoa, apparatus, method, or procent diaclound in the reports
Ag unod to the above, "period acting on behalf of the Commissions includes may m-
ploya or contructor of the Commission. or employne of much contractor, to the extent that
such employee or contractor of the Corumission, or employee of mail contractor propurus,
disseminates, or provides access to, aay Information pursuant to do employment or contract
with the Commission, or no employment with such contractor.
errae I
ORNL-DWG 66-3214
los
TNBS NO. 442
16--2---NBS NO. 443
EXPOSURE (mou coulombs)
.
OE-NBS NO. 444
NBS NO. 1178
102
10°3
i
r
- -
-
*
10-3

105
102 101 100 100 10² 103 104
BORON (w! ppm)
Boron in Steels - NBS Standards ("B at 40% Transmittance.)
slide I
ORNL. DWG. 66-4510
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6 2.
7
7
7
.
....
.
MIRCENT TC N Cr-TC ALLOYS
Amoy A B C
Taschen
(Direct Reader) 3.5 9.3 16
VS-7
(Spark Source) 2.1 8.7 15
-:
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nemitissimo
*********************
..
.
.
.
-
-
-
..
.
- -
-
-
-
-
-
.
.
-
.
.
-
.
-.
.-
-
PA*
*
i slide II)
ORNL DWG. 66-5868
Element
Added
Found
A1
100
900
SOLUTION RESULTS BY MS-7
(Wt. ppm)
Cr Fe, Mn Ni
100 100 100 100
110 110 150 78
Remarks
U Matrix -
Nb Substrate
Added
Found
10
9.1
10
9.1
10
12
.
10
10
10
7.8
.
Solution -
Nb Şubstrate
Added
Found
1
1.4,
1
0.9
1
0.6
1
0.6
1
0.5
a
Solution -
Au Substrate
Sr as internal standard
---,--.
-
-come.
- T
anrı
TABLE I
Distribution of Radioactivity In Source
Source Part
First slit
Electrode Clamps
Shield
% Present
90.0
7.5
1.7
0.4
Insulators
Kidney Plate
Window
Walls of Source
2nd Slit
0.2
0.1
0,1
Nil
3rd slit
Nil
Plate
NIL
TIDL: II
rinalysis oi' Irradiated
Corrosion Products
(Weight %)*

Sample
2.?
23
10.03
0.28
1.2.
0.06
0.96
•
Ba
0.87
0.11
do
Br
0.02
0.03!
0,1
Bi
3.3
1.5
4.8
0.02$
Cd
Co
Nr.
0.5
0.008
4.7
0.05
0.12
3.0
2.1
19
1.7
0.55
Cu
XX
:
F
9.6
_
к
2.8
0.52
0.27
Li.
MO
1.5
1.0
, MO
2.3
0.13
0.09
0,05
0.09
0.03
Mo
0.18
Na
35
12
Ni
3.?
11.16
0.82
| 0.07
.
Pb
0.13
ļi Pt
.
.
.
Rb
-,-.
-
-
-
2.8
2.0
0.2
-
-
=
-
3.3
25
.
-
-
.
3.1
0.05
--:
4
-
.
0.6
—
th
Ta
:
:
.
2
-
1.6
0.101
> 31
Zn
28
0.036 0.05
0207
1.2
0.36
0.05
0.01 0.004
0.11
| 2.1
0.21 10.231
* Normalized
SPECTROGRAPHIC WORK FORM. COMMON ELEMENTS
UCN.8602
VENDO
il
ABLE III
Analysis of U
+ yь
Added
Found
2.0
1.9
0.60
0.52
0.20
0.27
A
.
.
.
,
END
DATE FILMED
7 / 21 /67








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