SOVIET ATOMIC ENERGY VOL. 42, NO. 3

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• Publication Date: September 1, 1977
• Content Type: REPORT

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Russian griginal VoL 42, No. 3, March, 1977
rc
September, 1977
SOVIET
ATOMIC
ENERGY
ATOMHAR 3HEPIVIR
(ATOMNAYA ENERGIYA)
TRANSLATED FROM RUSSIAN
CONSULTANTS BUREAU, NEW YORK
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SOVIET
ATOMIC
ENERGY
Soviet Atomic Energy is abstracted or in-
dexed in Applied Mechanics Reviews, Chem-
ical Abstracts, Engineering Index, INSPEC?
Physics Abstracts and Electrical and Elec-
tronics Abstracts, Current Contents, and
Nuclear Science Abstracts.
Soviet Atomic Energy is a cover-to-cover translaion of Atomnaya
Energiya, a publication of the Academy of Sciences of the USSR.
An agreement with the Copyright Agency of the USSR (VAAP)
makes available both advance copies of the Russian journal and
original glossy photographs and artwork. This serves to decrease
the necessary time lag between publication of the original and
publication of the translation and helps to improve the quality
of the latter. The translation began with the first issue of the
Russian journal.
Editorial Board of Atomnaya Energiya:
Editor: 0. D. Kazachkovskii
Associate Editor: N. A. Vlasov
A. A. Bochvar
N. A. Dollezhal'
V. S. Fursov
I. N. Golovin
V. F. Kalinin
A. K. Krasin
V. V. Matveev
M. G. Meshcheryakov
V. B. Shevchenko
V. I. Smirnov
A. P. Zefirov
Copyright 0 1977 Plenum Publishing Corporation, 227 West 17th Street, New York,
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SOVIET ATOMIC ENERGY
A translation of Atomnaya Energiya
September, 1977
Volume 42, Number 3 March, 1977
ARTICLES
Determination of Mineralization-Time from the Isotopic Composition
of Lead Sulfides ? G. E. Orclynets
Investigation of Uranium and Uranium-Containing Minerals by their
Luminescence Spectra ? B. S. Gorobets, S. S. Engoyan,
and G. A. Sidorenko
Facility for Intrareactor Investigations of an Aggregate of Physicomechanical
Properties of Materials by a Pulsed Ultrasonic Spectroscopic Method
? B. F. Anufriev, A. A. Balandin, V. M. Baranov,
and Yu. V. Miloserdin
Statistical Analysis of the Joint Effect of/Nickel, Copper, and Phosphorus on
the Irradiation Embrittlement of Pearlitic Steels ? A. A. Astaf'ev,
S. I. Markov, and G. S. Ka rk
Anion-Exchange Refinement of Plutonium and Neptunium Separated during
Extraction Reprocessing of VVER Fuel Elements ? V. I. Anisimov,
A. G. Kozlov, V. P. Lanin, A. K. Polunin, L. N. Fedotova,
and V. A. Shurmel'
Recrystallization of y- arid a-Hardened Commercial Uranium
? G. I. Tomson and Yu. I. Petrov
Apparatus for the Calibration of Film Dosimeters in Electron Radiation
Fields of High Intensity ? V. A. Berlyand, V. V. Generalova,
M. N. Gurskii, and A. P. Zhanzhora
DEPOSITED PAPERS
Spatial Distribution of d?d Neutrons ? D. V. Viktorov and T. S. Tsulaya
Calculations on the Energy Deposited in the Shield of a Fast Power Reactor
? V. A. Karpov, B. V. Koloskov, V. I. Matveev, and M. F. Troyanov. . . .
Theory of Neutron-Activation Measurements in Boreholes
? G. S. Vozzhenikov and Yu. B. Davydov
The Dose Distribution for a Thin Neutron Beam in a Tissue-Equivalent
Medium ? N. S. Budnikov and D. B. Pozdneev
Effects of Annealing on the Properties of Welded Joints between Uranium
? and Zirconium or Titanium Alloys ? V. R. Tatarinov, V. P. Ashikhmin,
and V. S. Krasnorutskii
LETTERS TO THE EDITOR
Anisotropy of Dose Sensitivity in Semiconductor Detectors of Varying
Construction Used for Dosimetry of Ionizing Radiation ? V. A. Manchuk
Dispersiveness of Radioactive Aerosols at the Novovoronezh Nuclear Power
Station ? S. S. Chernyi, V. P. Grigorov, V. I. Stepchenkov,
and V. N. Kirichenko
CONTENTS
Engl./Russ.
191 171
196 177
203 183
207 167
211 191
214 195
218 199
222 203
223 204
224 205
225 206
226 206
227 207
229 208
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CONTENTS
Titanium Alloys as Structural Materials for Liquid Metal Radiation Loops
(continued)
Engl./Russ.
? D. M. Zakharov
231
210
Use of Perturbation Theory for Experimental Study with a Pulsed Neutron
Source ? V. Ya. Pupko, V. A. Tarasov, and A. K. Sharapov .. .
233
212
X-Ray Spectrometer with an Si(Li) Detector ? M. Vidra
237
214
Flow Characteristics for Hot Water at an Initial Pressure of 22.8 MPa
Escaping into the Atmosphere ? D. A. Khlestkin, V. P. Kanishchev,
and V. D. Keller
239
216
Measurement of the Ratio between the Capture and Fission Cross Sections
of 239Pu ? V. P. Bolotskii, M. V. Polozov, A. N. Soldatov,
and S. I. Sukhoruchkin ?
?
242
218
Density, Surface Tension, and Viscosity of Melts of Uranium Trichloride with
Rubidium and Cesium Chlorides ? V. N. Desyatnik, S. F. Katyshev,
S. P. Raspopin, and Yu. F. Chervinskii
246
221
Some Yield Characteristics of Short-Lived Fission Products in A Sodium Heat-
Transfer Agent ?I. A. Efimov, Yu. V. Lopatin, L. I. Mamaev,
S. A. Stabrovskii, and V. S. Filonov
249
224
Electrical Resistance and Stored Energy in Low-Temperature Irradiation of
Titanium Diboride ? L. S. Topchyan, I. A. Naskidashvili,
V. V. Ogorodnikov, V. V. Petrosyan, and L. M. Murzin
251
226
Measuring the Temperature of the Neutron Gas with Solid-State Track Detectors
of Fission Fragments ? A. M. Bogomolov, A. D. Molodtsov,
and L. Ya. Tikhonov
254
228
A Light Flash Excited by a y-Quantum Pulse without Direct Visibility of the
Source ? A. V. Zhemerev, , Yu. A. Medvedev, and B. M. Stepanov
257
230
A High-Current Injector of a Linear Electron Accelerator ? V. A. Vishnyakov,
V. M. Grizhko, I. A. Grishaev, B. G. Safronov, and G. L. Fursov
231
High-Temperature Reactions between Zr + 1% Nb and Compacted Uranium Dioxide
? G. P. Novoselov, E. V. Komarov, and B. G. Pastushkov
262
233
COMECON CHRONICLES
.S---Seminar on Equipment and Operation of Reactor Systems of VvER Type
? G. L. Lunin
264
234
Thirty-First of the COMECON Standing Commission on Atomic Energy
? Yu. I. Chikul
265
235
Collaboration Notebook ...
266
235
INFORMATION
,...?/" New USSR Nuclear Power Stations ? E. P. Karelin
267
236
CONFERENCES AND MEETINGS
Conference of the American and European Nuclear Societies
? V. A. Sidorenko
270
238
-.-International Conference on Liquid Metal Coolants ? F. A. Kozlov
272
239
Third International Conference on Zirconium in the Nuclear Power Industry
? B. G. Parfenov
274
241
IAEA Seminar on Design, Manufacture, and Testing of Packaging Systems for Safe
Transportation of Radioactive Substances ? A. K. Sedov
278
244
Fifth International Conference on Current Trends in Activation Analysis
? I. N. Ivanov
279
245
Solar Processes and Solar Neutrons ? G. E. Kocharov
281
247
SCIENTIFIC?TECHNICAL COMMUNICATIONS
British Fusion and Plasma-Physics Research ? G. A. Eliseev
283
248
Processing and Storage of Radioactive Wastes in Canada ? V. D. Balukova
286
250
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CONTENTS
BOOK REVIEWS
Engineering Design of Nuclear Power Station Shielding ? Reviewed by
V. S. Yuzgin
The Russian press date (podpisano k pechati) of this issue was 2/24/1976.
Publication therefore did not occur prior to this date, but must be assumed
to have taken place reasonably soon thereafter.
(continued)
Engl./Russ.
288 252
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ARTICLES
DETERMINATION OF MINERALIZATION TIME FROM
THE ISOTOPIC COMPOSITION OF LEAD SULFIDES
G. E. Ordynets UDC 550.93
Isotopic analysis is being used successfully in the study of ore deposits. The results of isotopic studies
are being widely used for the solution of problems involving the age of ores and the source of ore materials.
The re is interest in the use of the isotopic-lead method for evaluation of the time of mineralization and for
refinement of the sequence of mineralization. For this purpose, an analysis was made of the lead in sulfides
of various ages from a hydrothermal uranium deposit in a uranium sulfide formation.
The deposit is located in the peripheral region of the central massif at the junction of two large tectonic
blocks. The enclosing rock is in the form of metamorphized precambrian amphibolites, gneisses, and mag-
matites containing seams of marbles and limestones with veins and intersecting dikes of pegmatites and aplites. The
15,5
15,0
71? 17,5 18,0 145 83 Pb/n4Pb
Fig. 1. Diagram of isotopic ratios of leads in
sulfides; +) analytic uncertainty; II) pyrite; III)
galena.
Translated from Atomnaya gnergiya, Vol. 42, No. 3, pp. 171-176, March, 1977. Original article sub-
mitted April 9, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
191
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TAlltat 1. Isotopic Composition of Lead Sulfide
Type of sample
204Pb,
208pb1207PbI, 208Pb,
1206pb/204pb1207Pb/284Pb
I2ospb/204pb 20epb/207pb aospbi207pb
208pb /(208Pb+
+207Pb)
Pyrite impregnated in
_ limestone
Recalculated
Pyrite impregnated in
limestone
Galena impregnated
in limestone
The same ,
Galena together with
quartz and sphaler-
ite in the zone of
crushing
Av. value for galenas
Pyrite scattered in
graphitized para-
gnetsses
The same
Pyrite in ground gra-
phitized material
of the cracked
zone (recalcu-
lated)
The same
Average value
Galena in carbon-
ate-polymetallic
vein (average of
two laboratories)
The satne
(ay. of two analyses
Galena in carbonate-
polymetallic vein
The same
(ay. of two analyses)
Galena in polyme-
tallic vein
The same
Average value
Galena in calcite
vein
Pyrite in calcite
vein
1,419 25,09 21 ,67 51,82
1,43224,61 21,6752;29
1 ,414 24,52 21,38 52,69
1,387 24,60 21,64 52,37
1,397 24,67 21,6852,25
1,393 24,70 21,63 52,28
1,389 24,83 21,57 52,21
1,392
1,358
1,384
1,378
1,370
,372
1,350
1,380
1,372
24,70
25,06
25,09
25,01
24,93
25,02
25,13
25,47
25,34
21,63
21,28
21,45
21,09
21,38
21,35
52,28
52,29
52,08
52,32
52,32
52,25
21,1852,34
21,35
21,16
51,80
2,13
1,363 25,39 21 ,21 52,04
1,342 25,28 21,22 52,16
1,35725,27 21,34 52,03
1,348 25,19 21,36 52,10
1,352 25,16 21,35 52,13
1,358 25,15 21,41 52,08
1 ,358 25,26 21 ,29 52,09
1,312
1,308
28,17
29,08
20,81
20,33
49,71
49,28
*Results recalculated by the Brown method.
Group I
17,68
15,27
36,52
1,158
2,391
1,11
17,19
15,13
36,52
1,136
2,413
1,13
17,34
15,12
37,26
1,147
2,464
1,14
17,74
15,60
37,76
1,137
2,420
1,13
17,66
15,52
37,40
1,138
2,410
1,13
17,73
15,53
37,53
1,142
2,417
1,13
17,88
15,53
37,58
1,151
2,420
1,13
17,75
15,54
37,57
1,142
2,417
1,13
Group II
18,09
15,37
37,75
1,178
2,457
1,13
18,13
15,50
37,63
1,170
2,428
1,12
18,15
15,45
37,97
1,175
2,457
1,13
18,20
15,60
38,19
1,166
2,447
1,13
18,14
15,48
37,88
1,172
2,447
1,13
Group III.
18,61
15,69
38,77
1,186
2,471
1,13
18,46
15,47
37,54
1,193
2,426
1,11
18,47
15,43
38,00
1,198
2,464
1,12
18,63
15,56
38,18
1,197
2,454
1,12
18,84
15,82
38,87
1,191
2,458
1,12
18,62
15,73
38,34
1,184
2,438
1,12
18,69
15,85
38,65
1,179
2,439
1,12
18,61
15,79
38,56
1,178
2,442
1,12
18,55
15,77
38,35
1,175
2,432
1,12
18,61
15,68
38,36
1,187
2,447
1,12
Group IV.
21,47
15,86
37,89
1,354
2,389
1,01
22,23
15,54
37,68
1,430
2,424
1,00
main ore-monitoring structures are large discontinuous tectonic zones of submeridional direction. As a rule,
they follow a course consistent with the enclosing rock and are traced over distances up to 20 km. The ore
bodies are coordinated with the near-meridional longitudinal tectonic zones and with the shallower dislocations
of northwesterly direction resting on them. In tectonic zones from 2 to 25 m thick, which are ordinarily in the
form of intensely crushed, graphitized, and pyritized fine-grained plagioclase-biotite gneisses, there appear
numerous veins of variously aged carbonates together with uraninites and selenides and impregnated-vein
uranium ores.
The geostructural and mineralogic features of the deposit were discussed previously [1, 2]. A study of
its mineral composition made it possible to pick out five successive stages of mineralization: graphite-pyrite,
quartz- pyrite, carbonate -sulfide, carbonate-chlorite -uraninite , and calcite-pyrite .
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TABLE 2. Results of Comparative Analy-
ses of Isotopic Lead Composition in Gal-
enas
Sample
no.
204Pb
288Pb
207Pb
208Pb
3
1,385*
24,46
21,57
52,58
1,389 t
24,73
21,71
52,17
11
1,352 *
24,99
21,03
52,63
L348t
25,25
21,37
52,03
Data of V. M. Eloev and A. S. Samoletov.
tData of Ya. Legierskii.
Only the sequence of formation of the concluding stages is established from direct geological observa-
tions. The age interrelations of the initial stages were established from general geological considerations
and by analogy with deposits in the region such as the age of uraninites, which is 270 million years [3-5].
To determine the isotopic composition of lead, samples of galenas and pyrites were collected from vari-
ous mineral complexes in the deposit. The lead was extracted with dithizone after acid leaching. Analysis of
the isotopic composition was performed on MI-1305 and MI-1311 mass spectrometers by the single-beam meth-
od using a silicate emitter. Four groups of lead-containing sulfides were picked out in accordance with geo-
logical location and isotopic composition (Table 1, Fig. 1).
Group I includes sulfides dispersed in limestones and belonging to the quartz?pyrite stage. The occur-
rence of this sulfide mineralization in Precambrian strata remains unclear; it is either metamorphogenic, asso-
ciated with metamorphosis of the enclosing rock, or is hydrothermal-metasomatic, resultingfrom the initial
stages of ore formation.
The pyrites 1 and 2, separated from samples of average-grain limestones, are almost indistinguishable
with respect to the isotopic composition of lead and occupy the extreme lower-left position in Fig. 1. A cor-
rection was introduced for contamination by uranium lead in the isotopic lead composition of pyrite 1 using the
method proposed by Brown [6, 7] based on the ratio 208pb/(206pb 4.2o7pb), which is usually 1.13 for ordinary un-
contaminated lead. On the average, this value corresponds to 52.37%208Pb and a deviation of I% is sufficient to
demonstrate contamination. One can assume that lead with a content less than 5290208Pb is contaminated by
uranium lead, and with a content greater than 52.75% by thorium lead. In pyrite 1, the concentration of 208Pb is
51.82%, which points to an admixture of uranium lead. The correction is introduced in the following manner:
dividing the value of 51.82 by 1.13, we obtain the percent sum of the uranium lead concentration
(206pb 207pb)
in the uncontaminated lead, which (45.86%) is 0.90% less than that actually measured in the sample (46.76%); we
subtract this excess of uranium lead (0.76% for 206Pb and 0.20% for 207Pb) from the corresponding measured
values (25.09-0.70 = 24.39% and 21.67-0.20 = 21.4770; we sum the resultant values with the concentrations of
20413b and 208Pb and take the sum (1.419 + 24.39 + 21.47 + 51.82 = 99.099) as 100% and then calculate the percent
content of each isotope in the corrected (recalculated) isotopic composition for lead. Figure 1 shows the values
of the recalculated isotopic composition of lead. A similar correction was introduced in the compositions of
pyrites 9 and 10. In pyrites 1, 9, and 10, the ratio 208Pb/(206Pb 207pb) was 1.10-1.11 before the introduction of
corrections, which indicates contamination with uranium lead. Luminescence analysis of the pyrites revealed
0.0004-0.0005% of uranium in them.
The maximum 204Pb content (1.41-1.53%) in pyrites 1 and 2 indicates the greatest age of the lead in these
minerals. According to J. Brown, a 204Pb concentration of 1.49% and above should correspond to Precambrian.
All the remaining parameters, particularly the 206Pb and 207Pb concentrations and the 206Pb?41313 and 20613b?,7Pb
ratios, correspond to a time between Precambrian and Fanerozoic. It canbe assumed that the lead in these
pyrites are Late Precambrian or Early Paleozoic. Lead of such an isotopic composition has not been known in
the region before now.
Galenas 3, 4, 5, and 6, which were collected in the same place as the pyrites discussed, are characterized
by identical lead composition within the limits. of error of the method and form a rather compact group in Fig.
1.
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TABLE 3. Model-Based Age of Lead Sulfides
Sample
no.
?
Isoto. ic ratio
Age, million yr
.0
xi
a.
a
z,
-..a-
a.
g
A
-
a.
a
.0
0
a.
a
1
1,136
2,413
360
340
? 2
1,147
2,464*
310
120'
3
1,137
2,420
- 360
310
4
1,138
2,410
350
360
5
1,142
2,417
330
330
6
1,151
2,420
280
310
Average for
Group I
1,142
2,417
330
330
7
1,178
2,457
140
150
8
1,170
2,428
190
280
9
1,175
2,457
160
150
10
1,166
2,447
210
190
Average for
Group II
1,172
2,447
175
190
11
1,186
2,471
100
80
12
1,193
2,426
60
280
13
1,198
2,464
40
110
14
1,197
2,454
40
160
15
1,191
2,458
70
140
16
1,184
2,438
110
230
17
1,179
2,439
140
230
18
1,178
2,442
140
210
19
1,175
2,432
160
260
Average for
Group III
1,187
2,447
100
190
?Not included in calculation of the average because
of anomalously high value for 208Pb content.
The isotopic lead composition of these samples shows that the sulfide mineralization scattered in lime-
stone is the oldest in the deposit. Furthermore, as follows from Table 1 and Fig. 1, the pyrites differ markedly
from the galenas in isotopic lead composition. It can be assumed that the formation of these sulfides was asso-
ciated with the initial hydrothermal-metasomatic process, probably in early Paleozoic time. The greater age
of the pyrite is apparently the result of the addition of Precambrian lead from enclosing formations.
Group II combines pyrites that form scattered impregnations in deformed and graphitized paragneisses of
the main tectonic zone. Although they also belong to the earliest graphite-pyrite stage, the formation of these
pyrites is associated with various mineral complexes that are spatially combined within the limits of the tec-
tonic zone. It did not appear possible to separate the analyzed pyrites from the tectonic zone with respect to
production; they were separated from crushed samples in the form of a 90-95% concentrate after washing with
methylene iodide.
As indicated above, some samples in this group (9, 10) are characterized by an increased uranium con-
tent (0.0004-0.0005%) and by an isotopic composition shifted in the direction of an excess of uranium lead. Re-
calculated results from the method of J. Brown are given for these samples in Table 1.
The isotopic lead composition is much the same for all pyrites in Group II. They form an independent
group differing markedly in isotopic composition from the sulfide of Group I. The average values for the
isotopic lead composition of these pyrites (206pb/204-,-
= 18.14; 20 7pb0 4pb = 15.48; 208pb/204,,,
= 37.88) can be
used as geochemical characteristics of their conditions of formation in the basic tectonic zones.
Group III contains the galenas 11-19. They were collected from northeastern veins, which are composed
of minerals of the carbonate-sulfide stage. Analytical results for galenas 16-19 were kindly furnished by Ya.
Legierskii.
In order to check the possibility of using the results from two different isotope laboratories, parallel
analyses were made of the isotopic lead composition in two galenas (Table 2). The results were in satisfactory
agreement with the best being those for the determination of 204Pb.
Despite some spread in the data resulting from varying material composition of the veins, their differing
thicknesses, and the effect of enclosing rock, we note that the isotopic lead composition of the galenas in Group
III varies insignificantly. These samples form an isolated group in Fig. 1. Galenas 12 and 13 differ slightly
194
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Declassified and Approved
from the others. In them, the 204Pb
207Pb, and 208Pb to 204Pb are a little
be explained by the fact that in thin
of the enclosing rock has a greater
For Release 2013/04/01: CIA-RDP10-02196R000700090003-6
concentration is somewhat high, and correspondingly the ratios of 206Pb,
low in comparison with the average values. The higher 204Pb content can
polymetallic veins, where samples 12 and 13 were collected, the old lead
effect.
?
The galenas of Group III differ markedly from the sulfides of Groups I and II with respect to isotopic
lead composition and are characterized by a specific lead, the mean isotopic composition of which (18.61;
15.68; 38.36), corresponds to the Mesozoic age and can serve as a reliable isotopic characteristic of the car-
bonate?sulfide stage of mineralization.
If one assumes the age of uraninites to be 270 million years [4, 5], the disparity between the Mesozoic
age of the carbonate?sulfide stage and its position to the sequence scheme [2] before the carbonate?chlorite?
uraninite stage becomes obvious. The results are evidence of the fact that formation of carbonate?sulfide veins
occurred after carbonate?chlorite?uraninite veins. Therefore, the existing scheme for the sequence of miner-
alization requires refinement.
The galena 20 and pyrite 21, which were collected from the most recent veins, make up Group Iv. The
lead in these samples differs considerably from the preceding samples by reason of a marked excess of uran-
ium lead which is obviously anomalous. This appears most clearly in the markedly lower 204Pb concentrations
(around 1.31%), the anomalously high values for 206Pb (28-2a), etc. (Table 1). The isotopic lead composition
of these sulfides is evidence that buildup of radiogenic uranium lead (206Pb), which was captured by the most
recent sulfides concluding the hydrothermal process, occurred in the ore bodies of the deposit. Furthermore,
anomalies in the composition of lead sulfides are noted in the neighborhood of aggregates of uraninites of the
calcite?chlorite?uranium stage. Since the anomalous radiogenic lead was not observed at marked separation
from ore bodies, its use as a survey criterion, as was established in many uranium deposits of other types [8-
10], is obviously limited. The values of 208ptoo4ro?,
which are 37.89 and 37.68, do not differ from the values
corresponding to ordinary lead ore, which indicates the absence of high concentrations of thorium in the ores
because one would otherwise expect anomalously high values of this ratio in the lead of recent sulfides.
The results presented indicate that several types of lead are obviously distinguishable in the sulfides of
the deposit under consideration. Furthermore, each type corresponds to one or another period of mineraliza-
tion and is characterized by a definite isotopic composition which varies in regular manner from the oldest
lead of the early stages (Group I) to the youngest lead of the carbonate?sulfide veins (Group III). These data
are evidence of the pulsational nature of the hydrothermal-metasomatic process, each stage of which is charac-
terized by definite conditions for formation.
An attempt was made to determine the age of the lead in these sulfides from existing isotopic data. How-
ever, one should keep in mind that one does not ordinarily determine the age of mineralization from the iso-
topic composition of lead ore since it will depend on the model assumed for the evolution of lead in the earth's
crust. In addition, natural lead does not fall within the framework of the assumed model as a rule, and varying
isotopic ratios in a specific sample yield markedly divergent values for the age. Thus for the average isotopic
composition of lead in Hercynian deposits (about 150 samples), the age calculated by various methods varies
from 260 to 490 million years [4].
A model proposed by Legierskii and based on the use of 206Pb07Pb and 208Pb07Pb ratios [4, 5] was ac-
cepted for the calculation of the age of lead in the various stages of mineralization. The interpretation of the
resultant age values (Table 3) may not be unique. Nevertheless, it should be emphasized that the scattered
sulfide mineralization in limestone (Group I) is oldest (about 330 million years according to the calculation).
The age of the lead in the graphite?pyrite stage (Group II) is 175-190 million years. However, as already
pointed out, the pyrites were represented by several generations and the values obtained probably do not reflect
the true age of this stage. For lead in the galenas of carbonate?sulfide veins (Group III), the greatest spread
is noted in the age values calculated from the two isotopic ratios and the age of the lead in this stage of ore for-
mation is either Cretaceous (100 million years from the 206Pb/207Pb ratio) or Lower Jurassic (190 million years
from the 208Pb07Pb ratio) depending on the ratio accepted. In any case, acknowledge that the formation of
carbonate?sulfide veins occured in Kimmeridgian time.
The hydrothermal process of ore formation at the deposit studied continued for a period of 150-200 mil-
lion years and was accompanied by a regular variation in the isotopic lead composition. Each stage of mineral-
ization is characterized by an isotopic lead composition typical of it alone, which is a definite geochemical cri-
terion for mineral formation. The results of this work are evidence of the Kimmeridgian age of the carbo-
nate?sulfide veins and indicate the need for refinement of the existing scheme for the sequence of mineraliza-
tion, according to which the formation of the veins occurred in Hercynian time. Buildup of radiogenic lead,
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which was captured by the sulfides of more recent stages, occurred in the ore bodies. However, anomalous
lead sulfides were observed only in the immediate vicinity of the ore bodies or within them and therefore ob-
viously cannot be used as a survey criterion. Aging of the lead in pyrites of the quartz?pyrite stage, the ad-
mixture of Precambrian lead from enclosing gneisses in the galenas of thin polymetallic veins, and the re-
corded regularity concerning the unity of the source of uranium, vanadium, and selenium [2], are evidence
that the enclosing Precambrian formations may be the probable source of ore material.
The author is grateful to S. M. Eloev, A. S. Semoletov, and Ya. Legierskii for assistance with the work
and to V. E. Boitev and B. V. Brodin for valuable discussion of the materials in the preparation of the paper.
LITERATURE CITED
1. V. E. Boitsov and K. Stukhlikova, Izv. Vyssh. Uchebn. Zaved., Geol. Razved., No. 8,33 (1969).
2. V. E. Boitsov and Yu. M. Dymkov, in: Uranium Deposits: Zonality and Paragenesis [in Russian], Atomiz-
dat, Moscow (1970), p. 119.
3. A. V. Zavarzin et al., in: Uranium Deposits: Zbnality and Paragenesis [in Russian], Atomizdat, Moscow
(1970), p. 93.
4. Ya. Legierskii, Cas. Mineral. Geol., 18, No. 1, 1 (1973).
5. Ya. Legierskii and M. Vanacek, Acta Univ. Carol. Geol., No. 2, 153 (1967).
6. J. Brown, in: Lead Isotopes in Ore Deposits [Russian translation], Atomizdat, Moscow (1969), p. 194.
7. J. Brown et al., in:Lead Isotopes in Ore Deposits [Russian translation], Atomizdat, Moscow (1969), p.197.
8. R. Cannon et al., in: Geochemical Surveying [Russian translation], Mir, Moscow (1973), p. 228.
9. D. Ya. Surazhskii and A. I. Tugarinov, At. Energ., 9, No. 1, 21 (1960).
10. A. I. Tugarinov et al., At. Energ., 25, No. 6, 483 (1968).
INVESTIGATION OF URANIUM A ND URANIUM-CONTAINING
MINERALS BY THEIR_ LUMINESCENCE SPECTRA
B. S. Gorobets, S. S. Engoyan, UDC 535.372:549.755.35
and G. A. Sidorenko
The photoluminescence of uranium minerals has been previously studied in [1, 2]. Exact spectra of 20
uranium minerals were determined, including the most widely distributed minerals, which luminesce at 77 and
298?K; these were the classes of phosphates, arsenates, silicates, carbonates, sulfates, molybdates, vanadates,
and hydroxides of uranium. The regular changes of the frequency values of completely symmetrical (c.$) and
asymmetrical (a.$) uranyl oscillations were established as a function of the anion composition of the ligands,
the presence in them of H20 and OH, and also the appearance of a relation between the type of symmetry of the
crystal field in which the uranyl exists and the ability of the latter to luminesce [1, 2]. The individuality of the
low-temperature luminescence spectra of uranium minerals of different crystallochemical groups was condi-
tioned by the diagnostic procedure of the many mineral types or their relations to a defined group, which con-
siderably facilitated the study of the oxidation zones of uranium deposits. The advantages were shown of the
luminescence method over other methods of phase analysis, involving its rapidity, the possibility of working with
milligram quantities, and the retention of the substances being analyzed in the original form.
The purpose of this paper is to determine and interpret the luminescence spectra of the rare uranium
minerals that have not been previously studied, so that the proposed procedure can be more versatile. The
problem also includes the explanation of the chemical bond effect on the luminescence of uranium, in particular
on the change of the light scale of the luminescence from bluish-green to red for Minerals of different classes.
Investigated Samples and Their Luminescence
Samples were successfully found and the luminescence was investigated of 20 previously unstudied uran-
Tranglated from Atomnaya Energiya, Vol. 42, No. 3, pp. 177-182, March, 1977. Original article submitted
May 19, 1976.
196
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of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
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5
17000 18000 19000 1c cm'
Fig. 1. Luminescence spectra of uranyl phos-
phates and arsenates at 298?K; 1) hydrogeneous
autunite; 2) sabugalite; 3) novacekite; 4) urano-
spinite; 5) sodium uranospinite.
17000 18000
19000 x, cm-'
Fig. 2. Luminescence spectra of uranyl phos-
phates and arsenates at 77?K; 1) hydrogeneous
autunite; 2) sabugalite; 3) novacekite; 4) urano-
spinite; 5) sodium uranospinite.
ium minerals and also four minerals containing uranium as an impurity.* All the mineral samples were exam-
ined beforehand by x-ray photography. The technique for determining the luminescence spectra is described in [1].
*The authors thank L. N. Belov, A. F. Buntikov, I. G. Zhirtsov, V. I. Ludikova, K. V. Skvortsov, A. A. Cher-
nikova, and co-workers of the Mineralogical Museum of the Academy of Sciences of the USSR for making the
samples of rare minerals available for our study.
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_
1
18000
----
17000 190 00 %, CM-1
Fig. 3. Luminescence spectra at 77?K. a)
Uranyl silicates: 1) Ca-ursilite; 2) (Mg, Na,
Ca)-ursilite; 3) sklodowskite; 4) soddyite.
b) Silica minerals: 1) chalcedony; 2) opal;
3) allophane; ----) luminescence at 298?K;
1298 :177 = 1 :10 (the spectra of all the miner-
als are identical).
Phosphates and arsenates related to the crystallochemical group of uranium micas: hydrogenous autunite
(3),* sabulgalite (1), uranospinite (1), sodium uranospinite (1), novacekite (2), and zeunerite (1), in principle,
gave the same type of luminescence spectrum as the previously studied minerals of this group, e.g., autunite
etc. (Figs. 1 and 2). In addition to the main series of equidistant lines I generated by the uranyl center I, in
which four molecules of "ordered" water occur, disordered uranyl centers II frequently appear; the nature of
the luminescence centers I and II in minerals with the autunite structure is considered in [1]. The very slight
shifts of the homologous lines of series I with the various representatives of the mica group, obviously, do not
always permit them to be reliably diagnosed, but in many times they may serve as additional diagnostic indi-
cators. Only for novacekite at 298?K is a clear difference observed from the other uranium micas: the clear
nonelementarity of the ko "lines." Series II, associated with disordered centers and appearing only at low tem-
peratures, likewise cannot serve as a mineral diagnostic, as its position varies both with the course of time
and also from region to region within the limits of the sample being studied (4I 19.500 ? 200 cm-1). The
weak luminescence of zeunerite at 77?K is similar to that previously observed for not quite pure torbernite
(phosphoric analog of zeunerite), contaminated with an autunite impurity [1]. Just like pure torbernite, pure
zeunerite should not luminesce, which is also mentioned in [2]. The weak luminescence, however, is due to
the intergrowth of zeunerite with another mineral, evidently uranospinite.
Arsenuranylite (found by L. N. Belov) was investigated. There is practically no difference between its
luminescence spectrum and the spectra of the phosphouranylite?renardite group of minerals, which are iso-
structural with arsenuranylite [1, 2].
Of the uranyl silicates (in addition to those previously studied in [1]), the following were studied: sod-
dyite, natural (1) and synthetic (more than 20), Ca-ursilite (2), (Mg, Na, Ca)-ursilite (2), sklodowskite (1), kazo-
lite (3), chevkinlite (2), and wichtisite (1). The last three minerals do not luminesce even at low temperatures,
which had been noted already in [2]. Uranyl silicates give similar (although not identical) luminescence spectra
within the bounds of their crystallochemical groups: 1) sklodowskite (Fig. 3a), boltwoodite, uranophane, 8- ura-
notil [1] (UO2:SiO4 = 1); 2) ursilite (UO2 :SiO4 1).1'
*The number of samples of the specified mineral is given in the brackets.
fPreviously studied samples of natural soddyite were found to be contaminated and their luminescence spectrum
cannot serve as a standard [1]. Seddyite, found by V. I. Ludikov, is taken as the standard, the luminescence
spectrum of which coincides with the spectrum of the synthetic mineral.
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TABLE 1. Spectroscopic Luminescence Characteristics at 77?K
Minerals
Uranyl electron-vibrational frequencies, cm-I
ko
ki
h 2
ha
k4, k5, k6
Ali s; [Aka]
Phosphates:
hydrogenous autunite
I. 20020
19160
18340
17500
16670,
830+5
H2(U 02 PO4 )2 ? 8112 0
19070
18250
17420
15860,
930-T-5
15070
sabugalite
I. 19940
19120
18320
17480 '
16660
820+5
HAI(UO2PO4)4 ?16H20
II. (19950)
(18800)
(18000)
?
(780)
Arsenates:
nocacekite
I. 19960
19140
18320
17420
820+5
Mg(UO2As04)2 ? 8H20
[19050]
[18250]
[17330]
[900+15]
II. 19640
18940
?
?
' (700)
uranospinite
I. 19890
19080
18260
17460
815+10
Ca(UO2As0s)2 ?(6-8).H20'
II. 19450
18780
?
?
(700)
sodium uranospinite
I. 19960
19120
18320
17480
16670
820+5
Na2(UO2As04)2(6-8).1-120
[19030]
[18230]
[17490]
?
[905+5]
II. (19520)
(18710)
(17930)
(17120)
(16360)
(780+20)
Carbonates:
andersonite
20790
19970
19140
18330
17490
825+5
Na2CCU02)(CO3)3] ? 61-120
[17420],
16690
[16600],
15870
19910
19050
18260
[15790]
[900+5]
rutherfordite
(19840)
(18900)
(18000)
(17200)
(16350)
(800)
UO2CO3
Silicates
soddyite
18730
18020
17300
16600
15890
710+10
(UO2)2(SiO4)?nH20
ursilites
19900
19100
18310
17520
(16700)
770+20
Cal(UO2)2(Si205)31?5H20
[19020]
[18200]
?
?
[890]
(Mg, Ca, Na)[(UO2)2(Si205)31'5H20
19570
18810
18050
17300
(16580)
760+20
sklodowskite
18780
18000
17260
(16600)
720+30
Mg[UO2(SiO3)01112 ? 5H20
Hydroxides and uranates
fourmarierite
18800
18050
17300
(16530)
750+20
Pb[(UO2)402(OH)6].4H20
becquerelite
18700
17950
17300
(16500)
730+20
Ca[(1j02)604(OH)61?8H20
schoepite I
18650
17920
17300
(16500)
750+30
UO2(011)2?H20
schoepite II
17550
16830
16100
(15400)
700-720
H2(UO2)02?H20 (?)
Uraniura-containing minerals
chalcedony SiO2
opal Si02.nH20
20000?
19200-1934018380-18550(17750)
(16900)
,825+5
allophane in mA1203
nSi02. pH20
calcites:
J 20180
single sample: phase I+
19570
18810
18050
17300
760+20
phase II (weakly)
19880
19150
18330
17580
780+10
three samples: phase II
18890
19160
18380
17630
16820
780+10
[19050]
[18230]
117530]
[16710]
[900]
Notes: 1. Accuracy of determination of the narrow lines ? 20-10 cm-1. 2. In the curved brackets ? frequencies
of the diffuse or "floating" bands, for which their center of gravity is shown approximately. 3. In the
square bracket? frequencies of the asymmetrical vibrations. 4. For brevity, the prefix "meta" is emitted
in the names of the uranium micas.
The uranyl carbonates were represented by andersonite (1) and anhydrous rutherfordine (1) . According
to the luminescence spectrum at 298?K, andersonite is no different from uranothallite, bayleyite, and schroeck-
ingerite M. However, these minerals are clearly different in the specific fine structure in the luminescence
spectra at 77?K (Fig. 4 and Fig. 3a and b of [1J). Rutherfordine does not luminesce at 298?K and even at a low
temperature the narrow lines of the fine structure are not observed in its spectrum, which confirms the greater
symmetry of the crystal field, in which the luminescence centers (uranyl) are located, in comparison with other
carbonates.
Hydroxides and uranates were represented by becquerelite (2), fourmarierite (4), schoepite (5), curite (1)
and elarkeite (1). The last two minerals do not luminesce even at 77?K, and the reasons for this still are not
explained precisely: becquerelite, fourmarierite, and two samples of yellowish-colored schoepite (schoepite I)
gave identical luminescence at 77?K (Fig. 5), which confirms the previously established fact of indistinguisha-
bility of the minerals within the bounds of the class of hydroxides as a result of the absence of a marked
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17000 18000 19000
20000
A; cm-'
Fig. 4. Luminescence spectra of uranyl car-
bonates and uranium-containing calcites at
77?K; 1, 1') andersonite at 77 and 298?K; 2)
rutherfordine; 3, 4) calcites from different
parts of the deposit.
15000 16000 17000 18000
Fig. 5. Luminescence spectra of uranyl
hydroxides and uranates at 77?K: 1) bec-
querelite; 2) fourmarierite; 3) schoepite
I; 4) schoepite II.
connection between the uranyl center of luminescence with the supplementary cations Ca2+ and Pb2+ [1]. Three
samples of schoepite, which had an orange color, at 77?K gave a bright red-orange luminescence with a pro-
nounced shift to the low-frequency region of the spectrum (see Fig. 5). This unusual color luminescence of the
uranyl minerals had not been observed previously. Its causes will be considered below.
Uranium-containing minerals also were studied; calcite (4), chalcedony (about 50), opal (about 40) and
allophane (5). An investigation of the luminescence spectra permitted the form of entry of uranium into the
mineral base to be established, which until recently was not precisely known. Uranyl does not occur iso-
morphically in calcites, but it is stored in the form of a finely dispersed impurity of the natural uranium mine-
rals. At least two such phases are exhibited, most likely belonging to Ca-ursilite and (Mg, Na, Ca)-ursilite
[see Fig. 4 (3,4) and Fig. 3 (1, 2)]. We note that according to [2], the low-temperature luminescence of the
uranyl in calcites is characteristic only for calcites with a low-temperature mineral formation.
For the oxides of the cryptocrystalline and amorphous group of minerals of silica, and also for alumino-
silicate (allophane), it was previously shown that aquacomplexes (UO2nH20)2+ adsorbed on the surface are the
predominant form of entry into them of uranium, where n = 4-6 [3, 4]. In this present paper, this conclusion
is confirmed by the investigation of about 100 samples of natural and synthetic silica that have adsorbed ura-
nium frora solution with a different anion composition. It was also established that the form of entry of the
uranium is identical for all the mineral types and varieties of this group; chalcedony, agate, cacholong, chryso-
prase, silica, opal, hyalite, and allophane of different color, taken from many deposits.
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TABLE 2. Dependence of Spectral Characteristics on the Chemical Bond in the Uranyl
Minerals
Class of minerals
ho, cm-1
Aks, cm-1
10-10 If,
force con-
stant. N/cm
Multiplicity
of bond, n
Luminescence
color
Nitrates [10]
204C'0-20S00
840-880
7,6-7,8
2,35-2,40
Blue-green
Carbonates
19900-20700
820-840
7,0-7,6
2,20-2,35
Azure-green
Adsorbed uranyl aquacomplexes in
19800-20100
820-830
7,0-7,3
2,20-2,25
Green
Si02
Phosphates and arsenates of the mica
group
19400-20000
810-830
6,8-7,4
2,15-2,25
Yellowish-green
Phosphates and arsenates of the phos-
phouranylite group
18750-18850
730
5,5
1,85
Yellow
Silicates
18700-19700
710-770
5,2-6,2
1,80-2,0
>>
Hydroxides
18400-18800
700-750
5,1-5,8
1,75-1,90
Yellow-orange
Uranates (schoepite II)
17500,-..---
680
4,8
1,65
Red-orange
Effect of the Chemical Bond in Uranyl Minerals on
the Luminescence Spectra
It is well known that with increase of basicity of molecules in the uranyl solvation or coordination sphere,
a shift occurs in the luminescence bands to the side of low frequencies [5]. This is due to an increase of the
chemical bond of the uranium atom with the ligands and a corresponding weakening (stretching) of the uranyl
bond U-01. As a result of this, contraction of the energy pattern of the uranyl electron-vibrational levels
occurs. The contraction of the uranyl vibrational sublevels in the excited state has been known for a long time,
in which the U-OI bond is longer than in the ground state; hence, the frequency of the completely symmetrical
vibrations of excited uranyl is less than for nonexcited uranyl; Al4 < Aks (see [6]). During stretching of the
uranyl, the electron levels of its ground and excited states, ko and 4, must converge in proportion with the
weakening of the uranyl bond in minerals of different classes. In this case, the frequency of the purely elec-
tron transition k ko is decreased, in consequence of which the color of the luminescence is shifted from the
greenish-blue to the red region of the spectrum. At the same time, the frequency of the uranyl completely
symmetrical vibrations is decreased from 800 to -700 cm-1 as a result of contraction of the ground state ener-
gy sublevels ko - nAks (Tables 1 and 2).
Knowing the length R of the U-01 bond and its force constant K, it is possible by Gordy's formula to esti-
mate the multiplicity of the chemical bond .n in uranyl:
K = 1.67n [(xux0)/R2]3/4+ 0.3, (1)
where xu = 1.9 and xo = 3.5 are the electronegativities of the U6+ and 02- ions. K can be calculated from the
luminescence spectra by the formula
K = 0.285 ? 10-6m0 {(Alc8)2 ? [mu/ (mo+ mu)] (Aka, (2)
where Aks and Aka are the frequencies of the completely symmetrical and the asymmetrical vibrationst; mo
and mu are the atomic masses of oxygen and uranium [6].
If the length of the bond is unknown from structural data, it can be estimated by Badger's formula [81:
R 1.08K-113 + 1.17, (3)
or by the formula proposed by Vdovenko et al. [9]*
R= 3.82?in (K+ 0.73).
(4)
tAka is determined either directly from the luminescence spectrum (see Table 1), or by the formula aka =
ks If 1 + 2m0/rav in cases when the asymmetrical vibrations do not appear in the spectrum in a clear form [6].
$The results obtained by Eqs. (3) and (4) are very close. The differences between them are important only for
chemically pure uranyl compounds, which give narrow stable lines. For minerals, the spread overlapping the
accuracy of the calculation is unavoidable and amounts to
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Calculations by Eqs. (1)-(3), using luminescence data, show how the multiplicity of the bond in uranyl is
reduced with increase of basicity of the ligand from 2.4 in nitrates (synthetic) to 1.8 in hydroxides (see Table
2).
Now we shall attempt to interpret the differences in the luminescence spectra of different samples of
schoepite. Taking account of the shift of ko by almost 2000 cm-1 during transition from schoepite Ito schoe-
pite II, and the reduction of the band multiplicity from 1.80 to 1.65, respectively, it can be supposed that two
structurally different forms of this mineral exist, despite the similarity of their radiographs. It is possible
that schoepite II is a transition form from hydroxides to uranates:-(UO2)(OH) 2n1-120 H2(UO2) 02 nH20. Ac-
tually, the large electronegativity of the 02- ligand in comparison with OH, the participation in the chemical
bond of H+ and H20 and, consequently, the possibility of the formation of hydrogen bonds between the uranyl
and ligand oxygens leads to a larger stretching of the uranyl bond in schoepite II and to a reduction of its
force constant in comparison with these same parameters in the hydroxides. It may be supposed that H+ exists
either in the form of oxonium H30+ in the cation sphere or as a proton between the uranyl and ligand oxygens,
forming hydrogen bonds.
The principal result of our work is the determination of the standard luminescence spectra of the majority
of uranyl minerals in a number of uranium-containing minerals. This has permitted us to suggest a new high-
speed method for their diagnosis, and also to explain the crystallocihemical characteristics of uranyl minerals
and to establish the form of entry of the uranium in "nonuranium" minerals. Taking account of the chemical
bond, an explanation has been obtained for the luminescence color shift from bluish-green to the orange-red
part of the spectrum, as a result of change of the anion composition of the uranyl minerals from carbonates to
hydroxides and uranates.
LITERATURE CITED
1. B. S. Gorobets and G. A. Sidorenko, At. Energ., 36, No. 1,6 (1974).
2. A. N. Tarashchan et al., in: The Construction and Properties of Minerals [in Russian], No. 8, Naukova
Dumka, Kiev. (1974), p. 107.
3. B.B. Gorobets and A. M. Portnoy, Zap. Vses. Mineral. Ova, No. 3, 357 (1973).
4. B. S. Gorobets et al., in: Radioactive Elements in Geological Processes [in Russian], Institute of Geo-
chemistry and Analytical Chemistry (GEOKIII), Akad. Nauk SSSR, Moscow (1975), p. 168.
5. G. I. Kobyshev and D. N. Suglobov, Dokl. Akad. Nauk SSSR, 120, No. 4,330 (1958).
6. E. Rabinovich and R. Belford, Spectroscopy and Photochemistry of the Uranyl Compounds [in Russian],
Atomizdat, Moscow (1968).
7. W. Gordy, J. Chem. Phys., 14, 305 (1946).
8. R. Badger, J. Chem. Phys., 3, 710 (1935).
9. V. M. Vdovenko et al., Dokl.?Akad. Nauk SSSR, 167, No. 6, 1299 (1966).
10. A. N. Sevchenko and E. I. Stepanov, Zh. Eksp. Tekh. Fiz., 21, No. 2, 221 (1951).
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FACILITY FOR INTRAREACTOR INVESTIGATIONS OF AN
AGGREGATE OF PHYSICOMECHANICAL PROPERTIES
OF MATERIALS BY A PULSED ULTRASONIC
SPECTROSCOPIC METHOD
B. F. Anufriev, A. A. Balandin, UDC 620.17+534-8
V. M. Baranov, and Yu. V. Miloserdin
The study of the changes of properties of reactor materials directly affected by intense radiation fluxes
in the active zone of a nuclear reactor is an important characteristic and is of scientific interest. Ultrasonic
spectroscopy methods are the most promising for measurements under irradiation, which can be used for in-
trareactor tests [1-3].
A method is proposed in [4, 5] for simultaneously measuring the elasticity constant (Young's modulus E
and Poisson's coefficient hi), the internal friction Q-1 and the dynamic hardness (HD according to Shore and the
dynamic yield point P according to Tabor) on a single sample of the material being studied. It is based on the
recording and subsequent analysis of the ultrasonic vibrations of the sample excited in it by a mechanical shock.
The structural simplicity of the measurement unit and the feasibility of using samples of small dimensions and
of simple shape allow tests to be carried out on materials under complicated conditions, which are charac-
teristic in the operation of nuclear reactors (hightemperature and intense radiation flux). In particular, the
properties of materials at high temperature have been investigated by this method [6, 7]. A facility will be
described later which is designed for the investigation of the changes of properties of structural and fissionable
materials under the action of radiation, at a temperature created as a result of the self-heating of samples in
the reactor core.
Fig. 1. Structural layout of the measurements; 1) sam-
ple being studied; 2) electromagnet; 3) small ball; 4)
sound-guide; 5) piezoreceiver; 6) reflector; 7) ampli-
fier; 8) high-frequency magnetic recorder; 9) pulse
shaper; 10) electronic recorder.
Translated from Atomnaya tnergiya, Vol. 42, No. 3, pp. 183-186, March, 1977. Original article submitted
August 7, 1975; revision submitted July 13, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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1
22
Fig. 2. Overall view of the measurement capsule
of the facility; 1) sample being investigated; 2, 11)
flanges; 3) clamps; 4) carrier tube; 5, 10) electro-
magnets; 6) tube-magazine; 7) branching; 8) plunger;
9) ball; 12) piezoholder; 13) piezotransducer; 14,
18) insulating bushes; 15) retainer; 16) shaft; 17)
rigid drawbar; 19) sound-guide; 20) reflector; 21)
thermocouple insert; 22) adjusting screw.
The principle of the measurement is illustrated by means of Fig. 1. The sample being studied, in the form
of a disk with diameter 14-16 mm and thickness 5-8 mm is placed on three needle bearings, so that its flat sur-
face makes a small angle (5-8?) with the horizontal plane. An electromagnet, which holds a small ball above the
upper surface of the sample, is positioned over the sample. One of the bearings serves as a sound-guide for
transmitting the ultrasonic vibrations of the sample to a piezoreceiver, outside of the active zone of the reactor.
A reflector is secured to the sound-guide, in the form of a plate which is parallel to the plane of the sample.
The ball, when dropped, impacts on the sample, causing it to vibrate at natural frequencies and thus, on re-
bounding at an angle to it, strikes the reflector and falls past the sample.
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TABLE 1. Results of Measurements of Young's Modulus, Poisson's Coefficient, Inter-
nal Friction, Heights of Drop of the Ball (Shore hardness) and the Dynamic Yield Point
of the Samples Investigated
Material
Young's modulus,
107 N/m2
Poisson's
coeff,
Internal friction
Drop Dynamic yield
height, cm point, 107 l\i/m7
Duralumin D16T
7760+80
0,340+0,006
(1,6+0,1)?10-3
12,6+0,3
96+3
7750
0,34
1,65?10-3
12,3
9-4-
7200
0,334
?
70-130
Steel 2ail8N9T
20700+200
0,280+0,005
(1,15+0,08)?10-3
11,6+0.3
138+5
21400
0,275
0,98.10-3
11,2
133
20000
0,28
? 10-3
?
130-180
Copper MZ
11600+100
0,335+0,006
(1,5+0,1)?10-3
6,0+0,2
42,0+1,5
11500
0,35
? 10-3
?
40-50
Note. For all materials the values given are in the first line obtained by the method developed, in the second
line the control data, and in the third line (but for copper in the second line) the handbook data.
The signals from the piezoreceiver, after amplification, are recorded by the magnetic recorder and fed
to the pulse shaper, which converts the high-frequency signals into square-wave pulses, andthen these are fed
to a device for measuring the time between the pulses.
By analyzing the vibrations recorded, the natural frequency of the sample and the decrement of the vibra-
tions can be determined, from which the corresponding elasticity characteristics (Young's modulus and Pois-
son's coefficient) and the internal friction of the material can be calculated. The natural frequency of the sam-
ple is determined by the increase of amplitude of the recorded signal, repeatedly reproduced on the screen of
an oscillograph with a filter-analyzer tuned to the corresponding frequencies. The values of two natural fre-
quencies of the sample are used to calculate the Young's modulus and Poisson S coefficient [8]. When the filter-
analyzer is tuned to one of the natural frequencies of the sample, the damping decrement is determined and the
internal friction is calculated.
By measuring the time interval between pulses, corresponding to the impacts of the ball on the sample
and the reflector, the dynamic hardness of the material (Shore hardness) [9] and the dynamic yield point (Tabor)
[10] can be calculated;
14 mg ( 1???
= [0. (hi _4 1,03 E
0505
)_4]1/5
E2
where h2 = (ha cos a ? d + gt2/2)2/2gt2 is the calculated possible height of recoil of the ball; ha is the distance
along the normal from the upper surface of the sample to the lower surface of the reflector; a is the angle be-
tween the horizontal plane and the plane of the sample; t is the time interval between impacts of the ball on the
sample and the reflector; hi in the height of drop of the ball; m is the mass of the ball; d is the diameter of the
ball; g is the acceleration of gravity; pi, 112, El, and E2 are the Poisson coefficients and Young's moduli of the
materials of the ball and of the sample, respectively.
The design of the intrareactor facility for the measurements by the method described has been developed
for use in the vertical experimental channel of the IRT-2000 reactor, which has a diameter of 52 mm and a
guaranteed neutron flux density of ?2 -1013 neutrons/(cm2 ? sec). The facility consists of the measurement sys-
tem, suspended on a cable in the experimental channel of the reactor, and a system for pumping-out and filling
the channel withhelium. The electrical leads and the high-frequency cables are brought out through the groove
of the shield plug and then through the flange of the channel to the upper platform of the reactor.
The design of the measurement system is shown in Fig. 2. The carrier unit of the structure consists of
three tubes with a length of 1.5 m of Duralumin secured by upper and lower flanges. On them are assembled
the unit for mounting the sample, combined with the sensor of the recording system and the unit for supplying
and dropping the balls. The sample being investigated is positioned on a flange by three bearings and is tight-
ened with clamps. One bearing is the sound-guide and another is an adjusting screw, by means of which the
required inclination of the sample can be set; the third one serves as the junction of a Chromel?Alumel ther-
mocouple, the insulating sleeve of which is rigidly fixed into the flange. The reflector is fixed on the molyb-
denum sound-guide with a diameter of 3 mm. The rod sound-guide, with a length of 1.5 m, is insulated from the
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7
12
-11
5 -10
u,
E
3
O.
273 475
673 T,
Fig. 3. Temperature dependence of Young's
modulus, Poisson's coefficient, internal fric-
tion, and dynamic yield point of copper, grade
MZ (E* are the handbook data).
walls of the carrier tube by fluoroplast bushes. The piezotransducer, TsTS-19 ceramic with a diameter of 8
mm and height 15 mm, is located in a holder outside the active zone of the reactor.
The unit for supplying and releasing the balls of magnetic material is located in the upper part of the
measurement system. The magazine, in which 100 balls are placed, is a curved tube with an internal diameter
of 3.5 mm, fixed into the flanges of the upper and lower electromagnets.
When there is no current in the winding of the electromagnet, the lower ball in the magazine is in the
groove of the disk plunger with a diameter of 24 mm and thickness 3 mm, fixed on the axis in the branching.
When a voltage is applied, the shaft with a step rotates the plunger through the drawbar and releases the ball
which, under the action of its own weight, rolls down through the tube into a recess where it is held by the
switched-on electromagnet. The ball is dropped when the power supply of the lower electromagnet is cut off.
The pumping-out and filling of the system with helium consists of a mechanical and a diffusion pump, a
helium flask, vacuum valves and conduits with a length of 10 m and an internal diameter of 20 mm. After
several successive pump-outs and purgings, it provides a residual air pressure of ?10-4-10-5 mm Hg.
The principal technical data of the facility are defined by the following parameters. Operating range of
temperature up to 900?K. The indentors are tempered balls of ShKh-15 steel with a diameter of 3 mm. The
drop height is 300 mm. The measurement error of the natural frequencies of the sample, with a confidence
coefficient of 0.95, is 0.05-0.07%, which has been established by repeated measurements of samples of different
materials and by comparison of the results obtained with the data from parallel measurements by a resonance-
pulse method [111. The error in determining the relative changes of Young's modulus and Poisson's coefficient
is 0.1-0.15%. The error in calculating the absolute values of E from the natural frequencies of the sample (tak-
ing account of the error in measuring the sample dimensions, determining the density, etc.) does not exceed
1%, for Poisson's coefficient it is 2%, and for the internal friction it is 7-8% [6, 71. The error in measuring the
time intervals between impacts of the ball at the sample and at the reflector is not higher than 1.5% (with a con-
fidence coefficient of 0.95), and consequently the error in determining the Shore hardness is ~370 and for the dy-
namic yield point it is ?3.5%. The temperature of the sample during self-heating was determined with an error
of 5-7?K. The facility can be used also for the prereactor investigation of materials over a Wide range of tem-
peratures, for which a special cryostat and a high-temperature furnace have been developed 131. Table 1 shows
the results of measurements on samples of Duralumin D16T, stainless steel Ich18N9T, and copper MZ at room
temperature under laboratory conditions. For comparison, the results also are given of control measurements
of these properties (the constants of elasticity and internal friction were measured by the resonance-pulse
method 1111, the dynamic hardness by a photoelectric method [9]), and the handbook values [121.
Figure 3 shows the temperature dependence of Young's modulus, Poisson's coefficient, internal friction,
and the dynamic yield point of samples of copper M7. The small peak of the internal friction at 510?K
is due to viscous slippage along the grain boundaries [13]. The data obtained coincide well with [12],
13]. Measurements on samples of fissionable materials under laboratory conditions at 100-800?K and under
Irradiation in the active zone of the IRT-2000 reactor over the temperature range 350-800?K confirm the pro-
spects of the procedure described.
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LITERATURE CITED
1. Yu. V. Miloserdin, V. M. Baranov, and K. I. Molodtsov, At. Energ., 32, No. 4, 330 (1972).
2. V. M. Baranov, A. V. Rimashevskii, and V. N. Kakurin, Methods and Means of Investigating Materials
and Structures Operating under the Effect of Radiation [in Russian], No. 1, Atomizdat, Moscow (1973),
p. 62.
3. Yu. V. Miloserdin et al., At. Energ., 35, No. 2, 101 (1973).
4. V. M. Baranov, Yu. V. Miloserdin, and V. M. Shchavelin, Byull. Izobret., No. 34 (1970).
5. B. F. Anufriev, V. M. Baranov, and Yu. V. Miloserdin, Nauchn. Tr. Vyssh. Uchebn. Zaved. Lit. SSR,
Ul'trazvuk, No. 3 , 31 (1971).
?6. Yu. V. Miloserdin, B. F. Anufriev, and V. M. Baranov, Zavod. Lab., 37, No. 7, 977 (1971).
7. B. F. Anufriev and V. M. Baranov, Problems of Procedure and Technique of Ultrasonic Spectroscopy
[in Russian], Kiev Polytechnic Institute, Kaunas_ (1973), p. 101.
8. V. M. Baranov, Zavod. Lab., 38, No. 9, 1120 (1972).
9. A. A. Kurbakh, V. M. Shavelin, and N. A. Evstyukhin, Metalloceramic and Refractory Materials [in Rus-
sian], Moscow Engineering Physics Institute, Moscow (1967), P. 29.
10. D. Tabor, Hardness of Metals, Clarendon Press, Oxford, England (1951), p. 112.
11. V. M. Baranov and Yu. V. Miloserdin, Methods of Investigating Refractory Materials [in Russian], Atom-
izdat, Moscow (1970), p. 61.
12. I. V. Kudryatseva (editor), Materials in Machine Construction. Handbook [in Russian], Vols. 1 and 3,
Mashinostroenie, Moscow (1967).
13. M. A. Krishtal, Yu. V. Piguzov, and S. A. Golovin, Internal Friction in Metals and Alloys [in Russian],
Metallurgiya, Moscow (1964).
STATISTICAL ANALYSIS OF THE JOINT EFFECT OF NICKEL,
COPPER, AND PHOSPHORUS ON THE IRRADIATION
EMBRITTLEMENT OF PEARLITIC STEELS
A. A. Astaf'ev, S. I. Markov, UDC 621.039.531:669.15
and G. S. Kark
A considerable amount of experimental data has been published on the radiation stability of steel used in
fabricating elements for atomic power plants. However, the laws obtained are not, as a rule, of a general
nature and describe only special cases of the effect one parameter or another has on the radiation stability of
a material.
Attempts have recently been made to take account of the combined effect of several parameters on radia-
tion stability. It has been discovered [1] that at an elevated irradiation temperature the presence of nickel and
copper in ferritic?pearlitic steel 48TS leads to irradiation embrittlement. At a quite low impurity concentra-
tion no undesirable influence by nickel and copper was detected. It is pointed out [2] that impurities such as
phosphorus have a much more pronounced effect on irradiation embrittlement at an elevated than at a low (50-
80?C) irradiation temperature; at an elevated temperature nickel reduces the radiation stability of steel, evi-
dently by amplifying the embrittling effect of phosphorus.
Information about the deleterious influence of copper and phosphorus on the radiation stability of steel is
contained in a number of other papers as well, but unfortunately, there are no quantitative estimates of the joint
effect of these elements and the relation between their effects and the nickel concentration.
A multifactor experiment allows such an estimate to be made. In the present paper an attempt is made to
simulate such an experiment by statistical analysis of a large number of published data about the effect of the
chemical composition of pearlitic steels on their radiation stability.
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 187-190, March, 1977. Original article sub-
mitted March 19, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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The initial information was collected from??=?? 200 sources, primarily American, British, and Canadian
publications devoted to problems of reactor materials as well as from the materials of international confer-
ences and symposia.* The overall volume of the material collected comprised more than 1000 experiments,
in each of which 10-15 factors and 5-15 output parameters were recorded.
To accomplish the task set, viz., to evaluate the combined effect of copper, phosphorus, and nickel on the
irradiation embrittlement of steel, we selected those experiments (230 in all) that gave the chemical composi-
tion of the steel (including the copper and phosphorus concentration), the irradiation conditions (fluence and
temperature), and the characteristic of irradiation embrittlement, i.e., an increased temperature of the brit-
tle-ductile transition of steel (AT& as a result of irradiation. The heat-treatment parameters of the steel
were not introduced into the analysis as factors, but the sampling corresponded to roughly one level of these
parameters. Such factors as the reactor type, the neutron spectrum, and the size of the blanks for the samples
were not taken into account; this, of course, resulted in a random spread of the experimental data with respect,
to the mathematical model constructed.
Tabulated below are the maximum, minimum, and mean contents (in%) of alloying elements and impuri-
ties in the chemical composition of the steels analyzed;
C . .
. 0.26;
0.02;
0.18
P . .
. 0.045;
0.004;
0.013
Si .
. 0.41;
0.11;
0.24
S . .
. 0.05;
0.004;
0.019
Mn .
. 1.63;
0.40;
1.18
Cu.
. 0.35;
0.005;
0.19
Cr .
. 1.83;
0.02;
0.85
V . .
. 0.09;
0.005;
0.04
.
. 3.28;
0.01;
0.78
Al . .
. 0.06;
0.02;
0.035
Arlo .
. 0.6; 0.003;
0.30
The fast-neutron fluence with E > 1 MeV is 5.1018-102? neutrons/cm2 and an irradiation temperature of
250-350?C. For a lower irradiation temperature such analysis should evidently be carried out separately since,
according to the data of [2] and a number of other papers, embrittlement in this case is governed by other laws.
The mathematical apparatus of statistics was used to determine the character of the influence of one fac-
tor or another on LITK, to construct empirical equations (regression equations) describing the dependence of
ATK on the factors, as well as to verify the significance of the coefficients in the equations and the adequacy
of the statistical models. The statistical parameters were calculated on an M-220 computer.t
Possible mathematical models were constructed in the form of the regression relation
11
AT?=_- ao -FE aixi+1 a1x1.-+ J auxixj,
1, J..i
(1)
where xi are the influence factors; ai and aij are regression coefficients; i, j = 1, 2, ..., n; i j; and n is the
number of factors.
The criterion chosen for comparison of the various models was that of the residual variance of the ex-
perimental values of ATK with respect to the regression equation. It turned out that the optimal mode, i.e.,
the one having the minimum residual variance with terms of no greater than second order, was a statistical
model of the form
AT,- 110- 1224 [C12- 76 [Nil + 129 [Cu] + 4543 IN + 164 [Ni] [Cu] - 10320 [Cul 71 irr. (2)
where the chemical symbol in brackets denotes the concentration of the element; F is the fluence ,$ 1019 neu-
trons/cm2; and Tirr is the irradiation temperature, ?C.
The regression equation obtained is significant since it -reduces the residual Variance by a factor of
4.26, which exceeds the tabulated value of the Fisher test (4) = 1.60) for the given number of experiments and
determined coefficients at a significance level of 0.99.
Verification of the significance of the regression coefficients has shown that the coefficients in front of
the [Mn], [Si], [Cr], [Mob and [S] terms are either insignificant or at the significance limit; therefore, they
*This information was collected and systematized by V. A. Yukhanov, A. N. Tarasova, V. A. Nechaev, and G. F.
Prokoshina.
tN. N. Panichkin took part in the calculations.
$In the quite narrow range investigated, 0.5 4019-1020 neutrons/cm2, the effect of the fluence on ATI< is des-
cribed by a linear relation with satisfactory accuracy. In constructing a model for a broader range of fluence
values, it is desirable to use more complex relations such as TKn Ft/nor ATK log F+C, which havebeen-
given in the literature.
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3,0
2,4
48
140150 180 210 240
40
2,4
1,8
1,2
46
0 406 412 418 424 450
406 472 418 424 go
Copper content, %
Fig. 1. Two-dimensional section of model dia-
gram of irradiation embrittlement of reactor
pressure-vessel steel (the numbers next to the
curves denote the values of ATK, ?C).
have not been incorporated into Eq. (2). The conclusion that these elements exert a weak influence is, in the
main, in agreement with the data of one of the most detailed investigations on the effect that alloying elements
have on the radiation stability of iron?carbon alloys [3]. The authors of that paper show that in the case of
irradiation at 300-350?C a change in the manganese, chromium, and molybdenum content does not affect the
sensitivity of the material to radiation embrittlement. It was also shown [4] that at this irradiation tempera-
ture manganese at not does have any effect. Concerning the influence of molybdenum, V.I.BadaninandI.ARazov
[3] note that an addition of ?0.2% molybdenum enhances the radiation stability of iron?carbon alloys but this
stability remains unchanged as the molybdenum concentration rises further to 1%. In Eq. (2) the coefficient in
front of [Mo] proved to be insignificant, probably because the overwhelming majority of reactor pressure-ves-
sel steels analyzed contained molybdenum in quantities exceeding the threshold quantity.
In analyzing a statistical model, particular attention should be paid to the terms characterizing the effects
of interactions, i. e., [Ni] [PI, [Ni] [Cu], and [Cu] [P]. Initially, the various possible interactions between pairs
in the model were verified: [Nil [s], [Cr] [C], [Ni] [Cr], [Ni] [P], etc. However, only the products [Nil [P], [Ni]
[Cu], and [Cu][P] significantly reduce the residual variance, i.e., affect ATK. This means that the influence of
nickel on the radiation stability of steel depends on the quantity of phosphorus and copper in steel, and even the
character of this influence (increasing or decreasing 6.TK) may differ at different concentrations of phosphorus
and copper.
It is interesting that taking account of the effect of the interactions of nickel with phosphorus and copper
not only reduces the residual variance but also significantly changes the coefficient in front of [Ni] which is
+47.0 without allowance for the interactions and which, when these interactions are taken into account, changes
sign and takes the value ?76.0. This gives rise to a very important conclusion about the fact that in a number
of experiments there has been a tendency for ATK to increase with the nickel concentration, this being due not
to the influence of nickel itself but to its interaction with copper and phosphorus and occurring only at some
critical concentrations such that the positive sum of the contributions of the interactions of nickel with phos-
phorus and copper is greater than the negative contribution of [Ni] to ATK.
Unfortunately, this result cannot yet be compared with published data since practically no information is
available about the systematic study of the influence of nickel on the irradiation embrittlement of reactor-vessel
steels with a high concentration of phosphorus and copper. Data are available about the influence of nickel on
the behavior of steel with a low concentration of phosphorus, but with the copper concentration that is usual in
the commercial metal. Thus, increasing the nickel concentration in steel 15Kh2MFA with a phosphorus con-
centration of less than 0.01% does not intensify irradiation embrittlement [1] and is, therefore, desirable as well
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as allowable since it increases the margin of ductility-of the steel and its hardenability. The review [5] notes
that in order to explain the role of nickel in irradiation embrittlement it is necessary to investigate the influ-
ence at a low copper concentration.
Equation (2), obtained by statistical analysis, allows the influence of nickel to be predicted with the simul-
taneous reduction of the phosphorus and copper concentrations in steel (for example, 30% of the analyzed melts
contained less than 0.01% phosphorus and 0.1% copper). It is seen that as [P] and [Cu] decrease, the embrittling
effect of nickel decreases, to become neutral at some critical values of [P] and [Cu]. At an impurity concentra-
tion below the critical values, an increase in [Ni] decreases aTK. Therefore, analysis of the model (2) per-
mits the assumption that by reducing the copper and phosphorus concentrations in steel below the critical values
it is possible to reveal the favorable influence of nickel itself on the radiation stability and, by increasing its
content, to reduce ATK.*
Depending on the requirements imposed on the steel, (such as maximum allowable ATK, prescribed limits
of strength properties, etc.), all the critical concentrations can be determined by the techniques of nonlinear
programming and optimization.
For a graphic representation of the, combined effect of nickel, copper, and phosphorus on the irradiation
embrittlement of steel, a two-dimensional section has been built built of the seven-dimensional surface
corresponding to the model (2) (diagrams of irradiation embrittlement) for fixed carbon concentrations,
fluence, and irradiation temperature. The concentrations of elements were taken according to the data
of chemical analysis of a commercial melt of reactor pressure-vessel steel; the fluence and irradiation
temperature were taken to be 7 ? 1019 neutrons/cm2 and 290?C. On each section of the irradiation em-
brittlement diagram were lines of identical values of ATI( in coordinates [Nil - [Cu] for phosphorus
concentrations of 0.024, 0.015, 0.009, and 0.003%. The calculations were carried out on an M-220 com-
puter. The sections so constructed graphically illustrate the basis laws governing the combined effect of
nickel, copper, and phosphorus on ATK (Fig. 1). It is seen that at phosphorus concentrations of 0.024% and
higher (a) in the steel, nickel-increases the irradiation embrittlement over the entire range of concentrations
studied. At a phosphorus concentration of 0.015% (b) nickel intensifies the embrittlement of the steel only at
copper concentrations exceeding 0.06-0.0'7%. When the phosphorus concentration is reduced further (c), the
range of copper concentrations at which nickel is observed to have a favorable effect is extended and, along
with this, the magnitude of the shift of the temperature of the brittle-ductile transition, aTK, is decreased.
And, finally, at a phosphorus concentration of 0.003% (d), increasing the nickel content right up to 3% reduces
ATK practically over the entire range of copper concentrations allowable for the given steel (the lower the
copper concentration, the more effective the reduction). An increase in the nickel concentration to 2.0-2.5% at
[P] = 0.03% and [Cu] = 0.04-0.07% reduces ATK to 30-40?C. Raising the copper concentration to 0.2-0.25% even
with such a low phosphorus concentration increases ATK to 120-150?C.
Thus, analysis has made it possible quantitatively to evaluate the influence of nickel, copper, and phos-
phorus on the irradiation stability of steel, confirmed the earlier known fact that the radiation stability of
steel increased when it is purified of impurities, and showed that in this case a further margin of increase in
radiation stability lies in a possible increase in the nickel content (>1.5-2.5%), depending on the copper and
phosphorus concentration.
LITERATURE CITED
1. V. A. Nikolaev and V.1. Badanin, At. Energ., 37, No. 6, 491 (1974).
2. V. A. Nikolaev and V. I. Badanin, Izv. Akad. Nauk SSR, Met., No. 2, 126 (1975).
3. V. I. Badanin and I. A. Razov, Vopr. Sudost., No. 19, 92 (1975).
4. M. Brumovski, Author's Abstract of Dissertation, Moscow Engineering Physics Institute, Moscow (1971).
5. L. Steele, Neutron Irradiation Embrittlement of Reactor Pressure Vessel Steels, Tech. Rep. Ser. 163,
IAEA, Vienna (1975).
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ANION-EXCHANGE REFINEMENT OF P LUTONIUM
AND NEPTUNIUM SEPARATED DURING
EXTRACTION REPROCESSING OF VVER
FUEL ELEMENTS
V. I. Anisimov, A. G. Kozlov,
V. P. Lanin, A. K. Polunin,
L. N. Fedotova, and V. A. ShurmelT
UDC 541.183.5:546.799.4:546.799.3
When spent fuel elements from VVER reactors (water-moderated water-cooled) are reprocessed by ex-
traction with a 30% solution of tri-n-butyl phosphate in synthine at the stage of reduction re-extraction of plu-
tonium with uranium (IV), solutions containing the bulk of the plutonium and neptunium are formed [1, 21. The
plutonium and neptunium can be separated and their decontamination from uranium and fission products can be
completed by extraction [2] and sorption [3-5] methods. Of greatest interest is sorption with hexanitrate com-
plexes of actinides (IV) [6] on highly alkaline vinyl pyridine anion-exchange resins. References [5, 7] describe
the reprocessing of plutonium and neptunium concentrates from an extraction system for the regeneration of
spent fuel elements from an atomic power plant with a VVER-440 reactor by sorption of actinides on VP-1AP
anion-exchange resin with good technological characteristics.
The present paper gives the results of anion-exchange refinement of plutonium from a reduction re-ex-
tract from extraction regeneration of spent fuel elements from a VVER of the Novovoronezh Atomic Power
Plant with a 26-month cooling period (effective operating period 200 days). Sorption was carried out with an AB-
23M highly alkaline vinyl pyridine anion-exchange resin with a gel structure and a grain size of 0.4-0.6 mm.
The re-extract of plutonium and neptunium fed in for anion-exchange refinement contained 1.2 g Pu/liter,
0.09 g Np/liter, 0.5-8 g U/liter, and 0,8 M HNO3; the fission products were characterized by an exposure dose
rate (e .r.) of 0.45 ?R/(sec ? m2. liter). As a result of the high specific e.d.r. [- 375 ?11/(sec ? m2 ? kg Pu)] the so-
lutions were reprocessed according to a two-cycle flowsheet (Fig. 1).
In the process considered, an evaluation was made of how the method used to prepare the valence forms
Pu(IV) and Np(IV) affected their separation from the actinides and fission products in the stage of joint sorption
of Pu (IV) and Np(IV) in the first cycle and how the method of separation of Pu and Np affected the degree of
their mutual decontamination in the second cycle.
In the first cycle, joint sorption of Pu(IV) and Np(IV) was effected with 7.5 M HNO3; to obtain the required
valence forms of the extracted metal the initial solution was acidified to 7.5 M with respect to HNO3, and sub-
sequently had iron (II) and hydrazine nitrates added to it to a concentration of 0.2 and 0.1 M, respectively, [8].
The solution was allowed to stand for 45 min and then sent on for sorption.
TABLE 1. Characteristics of Solutions of I Anion-Exchange Cycle
Variant of
flowsheet
Charge, g/liter
Content, lo of initial
Comp, of desorbate
Extraction, 0/0
Pu
Np
filtrate
scrubbing
water
Pu,
g/liter
Np
mg/liter
U,
mg/liter
e.d.r.? 103,
PR/sec.
M2 .liter
Pu
Np
Pu
Np
Pu
Np
First
Second
14,3
14,3
1,1
1,1
0,6
0,9
1,2
4,1
0,1
0,1
0,7
0,4
3,57
3,56
286
262,5
12,0
5,0
4,4
3,5
99,3
98,9
98,6
94,8
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 191-194, March, 1977. Original article sub-
mitted April 9, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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Reduction re-ex-
tract Pu, Np
II cycle
Make-up
11NO3 7,5 M
Fe21- 0,2 M
N2114 0,1 M
H2C204 I g/liter
60?C
45 min
Sorption Pu (IV),
Np (IV)
Charge 15 g/liter
25? C
20 min
Scrubbing
HNO3 7 M
15 c. v."
-- 25? C
10 min
Desorption
Pu (IV), Np (IV)
HNO3 0,7 M
5 c. v.'
? 60? C
30 min
Desorbate
Pu (IV), Np (IV)
4 c. v.'
II cycle
Make-up
HNO3 7,5 M
NaNO2 10 g/liter
60? C
30 min
Sorption Pu (Iv)
Chale e- 13 g/liter
60?-C
30 min
Scrubbing
HNO3 7 M
20 c. v."
10 min
Desorption
Pu (IV)
HNO3 0,7 M
5 c. v.
? 60? C
30 min
Desorbata Pu (w)
2 c.
Filtrate
Reduction re-extract u, Np
I cycle
Make-up
HNO3 7,5 M
H202 0,2 Al
H2C204 I g/liter
70? C
60 min
Sorption Pu (IV), Np (IV)
Charge: 15 g/liter
? 25? C
20 min
Scrubbing
HNO3 7M
15 C. V.
? 25? C
10 min
Desorption Pu (IV), Np (IV)
HNO3 0,7 M.
? 60? C
30 min
Desorbate Pu (IV), Np (IV)
4 c.v.'
II cycle
Make-up
HNO3 7,5 M;
H2O2. 0,2 M;
? 70? C
60 min
a
Make-up
N2-114 0,2 M
85-90? C
60 min
Sorption Np (IV)
Change gluteni
?.25?C
20 min
Reduction
scrubbing
HNO3 5 M
Ascorbic acid
5 g/liter
5c. v.
?.25? C
20 min
Sorption Pu (IV), Np (IV)
Charge 15 g/liter
? 25? C
20 min
Scrubbing_
HNO3 7 M
15 C.V.
? 25? C
10 min
Desorption Pu (III)
HNO3 5 M
Ascorbic acid 5 g/liter
N2H4 0,1 M
? 25? C
30 min
Desorbatek Pu .(III)
2 C. v.
Scrubbing
HNO3 7,5 M
20 C. v,"
? 256 C
10 min
Desorption
Np (IV)
HNO3 0,7 M
Sc. v..
? 60 -?C
30 min
Desorbate
Np(IVI
5 c. v.'
Desorption Np (IV)
HNO3 0,5 M
5 C.V.
?60?C
30 rain
Desorbate Np tIV)
5 c. v.
? 'Colloidal volume of solution
Fig. 1. Flowsheet of two-cycle anion-exchange separation of plutonium and neptunium and their decontamina-
tion from uranium and fission products: a) first variant; b) second variant.
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TABLE 2. Characteristics of Solution of II Anion-Exchange Cycle
Variant cf.'
flowsheet.,E
C:11arge*
,,,-
g/liter
Content, To of initial
Comp. of desorbate '
Extraction,
6/0
Pu
Np
filtrate
scrubbing.
pffikl NI
reductio
scrubb
,..,
?
....7:
1,0
-Pu-
Np
Pu
Np
cr.cL,
Z to
..
U,
g/kg Pu
?
.?,.
iX =

a)
-du
Np,
mg/liter
Pu, 71
g/kg Np
g/kg ?Np ,
e.d.r., ?R/m21
sec ?kg Np
=
0.z
Np
e
z
Eqpt
Sorption
13,0
--
--
4,0
0,6
--
--
5,8
1,0
--
--
0,1
--
0,03
5,8
--
0,86
--
0,52
--
0,75
--
--
752,3
--
0,93
--
4,0
--
1,52
98,5
--
--
94,0
Second
13,2
0,96 0,08
1,3
0,09
1,6
--
5,9
0,81
0,5
0,28
186,0
26,9
16,1
5,9
98,6
95,9
TABLE 3. Coefficients of Purification of Plutonium and Neptunium from Each Other
and from Fission Products in Operations of Anion-Exchange Refinement
Cycle-
Variant
Decontamination factors
plutonium from
neptunium from
Np
fission
products
Pu
fission
products
First
1,96.103
3.102
1,27.103
3.102
Second
4,8.102
3,8-102
4,4.103
3,4.102
11
First
6,5
1.102
1,7
10,5
1,3.104
10
Second
2,8
1.102
3,5
1,2
5.102
2,3
Intwocycles
First
1,3.104
1.102
5-102
2,1.104
1,4-104
3.103
Second
1,3.104
1.102
1,3.103
5,3.103
5,5-102
7,9.102
In the second variant, Pu(IV)-Np(IV)couples obtained in a joint re-extract of plutonium and nePtunium
acidified to 7.5 M HNO3 were decontaminated with 0.2 M H202 [8].
After the sorbed metals were scrubbed from fission products with 7.5 M HNO3, plutonium and neptunium
were jointly desorbed with 0.7 M HNO3.
The desorbate of plutonium and neptunium was made up with HNO3 (to 7.5 M). Selective sorption was
carried out in the first variant. To obtain Pu(IV)-Np(V, VI) couples, sodium nitrite was introduced into the
acidified desorbate of the first cycle. After that, sorption of the plutonium (IV) was carried out and neptunium
remainded in the filtrate in quantity. After scrubbing with 7 M HNO3, the sorbed plutonium was desorbed with
0.7 M HNO3. The filtrate, containing neptunium, was treated with hydrazine nitrate.
Sorption of the neptunium (IV) took place at -25?C. For quantitative separation of neptunium and pluto-
nium the neptunium was subjected to reduction scrubbing with a 5 M solution of HNO3, containing ascorbic acid
and hydrazine. Once the sorbent had been scrubbed, desorption of the neptunium was carried out.
In the second variant, Pu(IV) and Np(IV) were sorbed jointly from the first-cycle desorbate of plutonium
and neptunium. After the sorbed metals were scrubbed to remove fission products, reduction desorption of the
plutonium was effected with ascorbic acid. The neptium was desorbed with 0.7 M HNO3.
The coefficients obtained for decontamination of the plutonium and neptunium from uranium, from all of the
fission products, and from each other in each cycle of the considered variants of the technological flowsheets
for anion-exchange refinement are presented in Tables 1-3.
When iron (II) was used to obtain Pu(IV)-Np(IV) couples in the operation of making up the solution before
the first cycle, the filtrate had a lower plutonium and neptunium content than when hydroxide peroxide was
used. In the first variant the values were 0.6 and 1.2%, respectively, and in the second, 0.9 and 4.1%, respec-
tively. With iron (II) the decontamination of plutonium and neptunium from uranium and fission products de-
creased (see Tables 1 and 3).
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The separation of plutonium and neptunium in the operation of plutonium (IV) sorption, when neptunium
(V, VI) remains in the filtrate (see Fig. 1), is more quantitative (separation factor -1.3 -104) than in the stage
of reduction elution of plutonium after joint sorption of Pu(IV) and Np(IV). The separation factor in this case
did not exceed -5 *102.
The principal decontamination factors are listed in Table 3.
The exposure dose rate of the plutonium desorbate in the first variant (0.745 pR/sec ? m ?kg Pu) was de-
termined from the radioactivity, in %, of: I44Ce + I44Pr 1.1; 106Ru 106Rh 3.6; 134C8 137CS 1.9; 95Zr 9.7; 95Nb 86; ?
in the second cycle (0.28 1.1R/sec ?m2?kg Pu), l44ce + 144pr 1.3; 106Ru + 196Rh 3.6; 134Cs + 137Cs 2.9; 95Zr 21.4;
95Nb 71.4.
With the gamma spectrum of plutonium taken into account, the factor of plutonium decontamination from
its various fission products in two cycles were: in the first variant, from 144Ce + I44Pr 2.2 '103; 196Ru + 196Fth
7.5 '103; I34Cs + I37Cs 2.7 ? 103; 95Zr 1.6 '103; 95Nb 2 "102; in the second variant 144Ce + 144Pr 3.8 *103; I99Ru +
I9611h 8.3 ? 103; 134Cs + 137Cs 6.1'103; 95Zr 1.9'103; 95Nb 6.102.
LITERATURE CITED
1. V. B. Shevchenko et al., in: Proceedings of the COMECON Symposium-Studies on the Reprocessing of
Spent Fuel, Vol. 1, Prague, Czechoslovak Atomic Energy Commission (1972), p. 259.
2. V. B. Shevchenko et al., Fourth Geneva Conference (1971), Paper USSR No. 435.
3. G. Burney and G. Thompson, Radiochem. Radioanal. Lett., 12, 207 (1972).
4. N. G. Chernorukov, in; Eleventh Mendeleev Conference on General and Applied Chemistry [in Russian],
Vol. 1, Nauka (1975), p. 270.
5. V. I. Paramonova, Radiokhimiya, 17, No. 6, 994 (1975).
6. E. D. Kiseleva and K. V. Chmutov, Zh. Fiz. Khim., 49, No. 8,2127.
7. V. I. Paramonova and N. B. Vysokoostrovskaya, Summaries of Papers on the Chemistry of Plutonium
[in Russian], Nauka, Leningrad (1975), p. 1.
V. S. Koltunov, Kinetics of Actinide Reactions [in Russian], Atomizdat, Moscow (1974).
RECRYSTALLIZATION OF - AND 8-HARDENED
COMMERCIAL URANIUM
G. I. Tomson and Yu. I. Petrov UDC 669.822.017
Comparison of the results of research on the recrystallization of hardened uranium, [1-4] and other
papers, shows that the recrystallization rate depends essentially not only on the impurity content, the a-an-
nealing temperature, and from what y or /3 range the hardening took place. Accordingly, studies were under-
taken on the causes of the different capacities of y- and 8-hardened uranium for recrystallization.
Research Material and Technique. The investigations were carried out on rolled specimens of commer-
cial-purity uranium measuring 2 x 10 x 30 mm. The content of impurities in uranium (mass %), 5 '10-2 C;
8 .10-3 Fe; 5 ? 10-3 Si; 4.10-4 Ni; 7 .10-4 Mn and 7 .10-4 Cu, did not exceed the solubility limit in the range.
Previously, the specimens were subjected to homogenizing annealing at 950?C for 2 h, followed by slow
cooling in a furnace (v
? - cool - 5 ?10?C/min). The specimens were heat-treated in a resistance furnace in quartz
ampuls with continuous evacuation (Pres - 2 *10-2 mm Hg). The temperature was measured by a PSP 1-60
potentiometer with a Chromel-alumel thermocouple.
The initial y and fi hardening was effected from temperatures of 950 and 740?C, respectively; after soaking
for 30 min, the specimens were cooled in water at 20?C. Brief heating of the specimens in the fi and y ranges in
Translated from Atomnaya gnergiya, Vol. 42, No. 3, pp. 195-198, March, 1977. Original article sub-
mitted April 30, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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j
?
Fig. 1. Structure of hardened and annealed uranium (x300): a) y hardening and 6 har-
dening (soaking for 30 min at 740 and 950?C, respectively); c) y hardening, 950?C, 30
min; c, d) y hardening +a annealing, 600?C, 4 h; e) fl hardening, 740?C, 30 min; e, g) fi
hardening +a annealing, 600?C, 4 h; etching: a, c, f) for a grain; b, e) for net; d, g) for
net and a grain.
the case of cross hardening was carried out in a bichromate bath. The duration of the heating was reckoned
from the time at which the required temperature (700 or 800?C, respectively) was reached on the specimen
surface; accordingly, thermocouples were fastened onto the specimens. Recrystallization annealing of har-
dened specimens took place at 600?C for 4 h. The a grains were exposed by electrolytical etching of electro-
polished sections at 40 V in a solution containing one part chromic acid to three parts acetic acid. The net
substructure of the impurity was exposed by chemical etching in a boiling mixture of equal volumes of nitric
and acetic acid.
The recrystallization was studied on the basis of data from metallographic analysis concerning variations
in grain size and shape.
Experimental Results and Discussion. Studies of the microstructure of specimens of uranium after har-
dening and annealing at 600?C for 4 h (Figs. la, c, and f) show that the recrystallization processes in y- and
6-hardened uranium do indeed proceed at different rates: 6-hardened uranium completely recrystallizes in that
time whereas in y-hardened uranium recrystallization has practically not started.
Possible slight differences in the grain and subgrain size and shape and in the magnitude and the inter-
nal stresses can scarcely account for the significant difference in the recrystallization rate of y- and fl-har-
dened uranium. However, etching for "net" shows that there are appreciable differences in the character of the
impurity distribution in y- and 6-hardened uranium (Figs. lb and e). Only quite large, uniformly distributed
inclusions are observed in 6-hardened uranium. In the main, these are carbides or hydroxycarbonitrides,
formed during the recrystallization process [1, 9, 10]. In addition to such inclusions, y-hardened uranium has
very fine inclusions (primarily carbides) and segregations of impurity atoms, forming a so-called net sub-
structure [6-8].
Impurities behave in different ways in y- and 0-hardened uranium and during the process of recrystalliza-
tion annealing. Fine, uniformly distributed inclusions as well as large ones were observed in 6-hardened
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Fig. 2. Structure of uranium hardened from 700?C (y-hardening +3-hardening) and an-
nealed (a-annealing at 600?C, 4 h); a, b) 30 sec; c, d) 1 min; c, f) 4 min (soaking at 700?C);
etching; a, c, e) for a grain; b, d, f) for net and a grain.
Fig. 3. Structure of uranium quenched from 800? (y-quenching+fl-quenching) and an-
nealed (a-annealing at 600?C for 4 h): a, b) 30 sec; c, d) 1 min; e, f) 4 min (holding
at 800?C). Etching: a, c, e) for a-grain; b, d, f) for net and a-grain.
uranium after annealing (Fig. if and g). In y-hardened uranium the original net substructure vanishes during
annealing (Fig. lb) and a large number of inclusions, forming a new net, appear along the boundaries of the a
grains and subgrains (Fig. lc and d).
Owing to the small strains that occur during the phase transformations and cooling in the a-range, re-
crystallization of the hardened uranium is evidently of a collective nature [5], i.e., individual grains and sub-
grains grow because of others; it is thus natural to assume that precisely the large numbers of inclusions that
are precipitated along the boundaries of a grains and subgrains and that block the motion of these boundaries
make recrystallization in y-hardened uranium more difficult than in a-hardened uranium.
Experiments with crossed hardening from the y and 13 phases have been carried out to determine how the
character of the impurity distribution in hardened uranium affects its capacity for recrystallization. These ex-
periments showed that heating of y-hardened uranium for a short time in the 13 range, followed by hardening,
sharply increases the capacity of uranium for recrystallization (Fig. 2a, c, and e), the increase depending on
the heating time in the f3 range.
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In the course of the heating in the ;3 range, the original net substructure of the y hardening is replaced by
a new net (Fig. 2b, d, and f); this new net is formed by inclusions that are stable at the 0-phase temperature
and changes little in the process of crystallization annealing. Even after short 30-sec heating in the g range,
there is a sharp drop in the number of inclusions formed during the subsequent recrystallization annealing
along the boundaries of the a grains and subgrains (Figs. id and 2b). As the heating time is lengthened the
number of these inclusions falls off even more (Fig. 2d and f). Thus, a definite correlation exists between the
capacity of hardened uranium for recrystallization and the number of inclusions formed along the boundaries
of the a grains and subgrains during annealing. The number of inclusions depends on the character of the im-
purity distribution and the stability of the net substructure in the hardened state.,
Brief heating of /3-hardened uranium in the range with subsequent hardening, by contrast, appreciably
reduces the capacity of uranium for recrystallization (Fig. 3a, c, and e), this reduction also depending on the
duration of the heating in the y range. The investigations have shown that a net substructure characteristic
of y-hardened uranium is formed in the process and, with subsequent recrystallizing annealing, a net of inclu-
sions is formed along the boundaries of the a grains and subgrains (Fig. 3b, d, and f). One can see clearly
that the number of these inclusions along the boundaries of a grains and subgrains grows as the duration of
the heating in the y range increases. Evidently, the quantity of impurities that goes over into the y-solid so-
lution increases, approaching the equilibrium concentration, and after hardening and annealing these impu-
rities can form inclusions of the other phase along the boundaries of the a grains and subgrains.
Thus, once again a connection is seen between the capacity of hardened uranium for recrystallization
and the character of its net substructure and, on the other hand, the number of inclusions formed along the
boundaries of a grains and subgrains during annealing. This confirms the assumption that the character of the
impurity distribution in hardened uranium has a predominant influence on its recrystallization.
LITERATURE CITED
1. A. P. Holden, Physical Metallurgy of Uranium [Russian translation], Metallurgizdat, Moscow (1962),
p. 147.
2. F. G. Foot, Metallurgy of Nuclear Power Engineering and the Effect of Irradiation on Materials [Russian
translation], Metallurgizdat, Moscow (1956), p. 89.
3. S. Push and B. Butcher, in: proceedings of the Symposium ? Reactor Technology, Select. Rev. (L. E.
Link editor), Oak Ridge, Tennessee (1964), p. 331.
4. A. Smith, J. Nucl. Mater., 26, 341 (1968).
5. S. S. Gorelik, Recrystallization of Metals and Alloys [in Russian], Metallurgizdat, Moscow (1967).
6. A. Robillard, D. Calais, and P. Lacombe, Rev. de Metallurgie, 55, No. 9, 815 (1958).
7. C. Angerman and R. Huntoon, J. Less-Common Metals, 9, No. 5, 338 (1965).
8. A. A. Bochvar etal., At. Energ., 27, No. 3, 193 (1969).
9. G. Ya. Sergeev, V. V. Titova, and K. A. Borisov, Physical Metallurgy of Uranium and Some Other Reactor
Materials [in Russian], Atomizdat, Moscow (1960)?
10. Ya. M. Sterlin, Uranium metallurgy [in Russian], Gosatomizdat, Moscow (1962).
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APPARATUS FOR THE CALIBRATION OF FILM
DOSIMETERS IN ELECTRON RADIATION
FIELDS OF HIGH INTENSITY
V. A. Berlyand, V. V. Generalova, UDC 621.387.46:541.15
M. N. Gurskii, and A. P. Zhanzhora
In several technological processes, materials are irradiated with intense beams of 200-700-keV elec-
trons. In such cases one must determine the dose absorbed in 100-500-?-thick organic material layers. Film
dosimeters can be used to measure the absorbed dose in rather thin layers and to determine the dose distribu-
tion over the depth of the object irradiated. Overheating by the radiation in the case of high dose rates (up to
107 rd/sec), active media (ozone,radiolysis products), and the possible accumulation of space charge in dielec-
trics [1] can substantially affect the dosimetric characteristics of film detectors. Therefore, when reliable
results are to be obtained with film dosimeters, the dosimeters must be carefully calibrated with the aid of an
absolute method, a calorimetric method, used under the real conditions of operation of the dosimeters.
The authors of [2-4] have described several calorimeters that are used to calibrate films at electron
energies in excess of 1 MeV. Little experimental work has been done on that problem at electron energies be-
low 1 MeV. Some of the work was reported in [5], where the measurements were made at electron energies of
0.3-0.5 MeV. The work by Dmitriev et al. [6] should be noted, because they calibrated polymethylmetacrylate
and polyvinylchloride films with the aid of a semiadiabatic total-absorption calorimeter. However, a method
of calibrating the detectors was nowhere described in full detail; the errors of the measurements were not
analyzed; and the dose rate range in which the calibration was made was either narrow or not indicated at all.
Description of the Calorimetric Apparatus. We developed in our work a calorimetric apparatus (see
Fig. 1) and a method of calibrating chemical film dosimeters in high-intensity electron radiation fields. The
main component of the apparatus is a calorimeter of the integral thermal flux; the calorimeter is operated un-
der stationary conditions and the electron beam incident upon it is completely absorbed. By using a calori-
meter of this type, one can avoid the difficulties resulting from temperature gradients inside the absorber of
?the calorimeter. In order to reduce the energy losses by bremsstrahlung and by backscattering of electrons,
the absorber of the calorimeter was made from materials with a low atomic number and was given the form
of a cavity. The absorber of the calorimeter is a combination of components: a graphite vessel with a wall
thickness of 1 mm is placed inside a thin-wall aluminum vessel whose external surface is coated with an oxide
layer. Calculations have shown that for an absorber of this type and this composition, the bremsstrahlung
losses at electron energies of 300 keV do not exceed 0.1%, whereas the losses resulting from backscattering
of electrons are below 0.6%. In order to calibrate the calorimeter with Joulean heat, a heating element of
manganin wire was inserted into the absorber. The heat flux which originates from the absorber of the calori-
meter is proportional to the rate at which under stationary conditions heat is liberated inside the absorber.
The heat flux is recorded with a thermopile comprising several thousand differential copper?constantan ther-
mocouples connected in series. A 10-p-thick aluminum foil prevents the convection of air. In order to reduce
the influence of temperature fluctuations in the surrounding medium, a differential scheme is employed: Two
identical calorimeters are connected in opposing relationship. During the measurements, one calorimeter is
exposed to the electron beam, whereas the other one is shielded by an aluminum shield. The calorimeters are
characterized by high thermal conductivity, low heat capacity, and, consequently, a small time constant (T = 25-
27 sec). The calorimeters were calibrated with a heat liberation rate of 10-3-10 W. The sensitivity of the
calorimeters was ?40 mV/W. The calorimeters are also electron collectors in the form of a Faraday cylin-
der. The calorimeters can be used to measure the electron flux and to determine the average electron energy.
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 199-202, March, 1977. Original article sub-
mitted May 10, 1976; revision submitted September 14, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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3
1 2
4 5 6 75.9
VZ
- ;
11
15
14
13
12 11 10
J
Fig. 1. Scheme of the calorimetric apparatus: 1) detectors; 2)
solenoid; 3) electron collector; 4) shutter; 5) collimator; 6)
shield with water cooling; 7) aluminum foil; 8) graphite foil; 9)
thermopile; 10) heater element; 11) foam plastic; 12) copper
block; 13) aluminum vessel; 14) motor; 15) disk-shaped drum.
During the operation of the accelerator, the fluctuations in the density of the energy flux of the incident elec-
trons can exceed 10-15%. It is therefore necessary to continually control the beam of electrons released. An
electron collector in the form of a ring was used as the monitor of the electron radiation. A collimator acts as
a diaphragm for the electron beam, which thereafter is incident either on the calorimeter to measure the flux
density of the electron beam energy or upon the detectors to be calibrated. The detectors are mounted in a
disk-shaped drum with 8 openings. The films exposed to the beam are shifted by remote control effected with
the aid of a motor. The required exposure to the radiation is obtained with a shutter which is operated by a
solenoid. A timer is connected in series with the solenoid. Thus, the time of irradiation can be fixed with
rather high accuracy (0.01-0.2 sec). A shield with water cooling is used to protect the entire apparatus from
the radiation.
A copper block and a layer of foam plastic reduce the influence of temperature fluctuations in the environ-
ment and guarantee uniform temperature conditions in the external shells of the calorimeter.
Calibration of Film Dosimeters. The film dosimeters are calibrated with a substitution method. At the
beginning, the flux density yo of the electron radiation energy is determined at a certain point with the aid of the
calorimeter. After that, film dosimeters are irradiated under the same conditions and the absorbed dose is
calculated. With the calculation method one can account for possible nonlinearities in the dependence of the
optical density of the films (or any other film parameters) upon the absorbed dose.
The calculations are made as follows. The relation between the readings of the total-absorption calori-
meter and the readings I of the monitor is established by several measurements:
= kI ,
(1)
where k denotes the proportionality factor.
The monitor signal I(t), which changes in the course of film irradiation, is recorded on the tape of an
automatic potentiometer. After integrating the function recorded over time, the readings of the monitor can
be used to determine the energy transfer of the electron radiation during the irradiation time;
to to
F = S (t)dt = k I (t)dt. (2)
At the beginning, several individual films are irradiated at given parameters of the accelerator. The ex-
posures are selected so that the entire range of absorbed doses to which the films may be exposed is covered
(the range is 2-25 Mrd in the case of cellophane). The energy transfer is determined for each film irradiated
and the optical density of the film is measured. The irradiation dose absorbed by the film is evidently directly
proportional to the radiatiOn energy transferred.
As a result of these operations one can plot a calibration curve in relative units, i.e., one can plot the
relationship between the dose absorbed by the film and some film parameter for which the ratio S/S0 is con-
veniently used (So denotes the optical density of the nonirradiated film). The error resulting from the spread
of the initial optical densities of the dosimeter films is then reduced (a being the proportionality factor):
up? f (S IS0). (3)
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4-2 49
48
"a")
47
46
;5
44
0
5 10 15 20 254 Mal
Fig. 2. Calibration curve S/S0 as a func-
tion of the absorbed dose of (x) electron
radiation and (0) y radiation.
The determination of a is the next problem. Por this purpose, a set of films which guarantee total ab-
sorption of the electron beam is irradiated and measured with a photometer. The coefficient a is obtained
from the normalization condition
miDi= E,
i=t
(4)
where mi denotes the mass of the i-th film of the total-absorption set, with the mass referred to unit area; n
denotes the number of films in the set; and E denotes the energy absorbed by the set of films, with the energy
referred to unit area. The absorbed energy is equal to the energy transferred minus the energy of the elec-
trons backscattered from the set of films:
E F (1? p),
(5)
where p denotes the albedo in terms of energy; in the case of cellophane, the albedo is 0.03 at an electron ener-
gy of 300 keV [7]. The energy spent on bremsstrahlung can be disregarded. We obtain with Eqs. (3)-(5):
E mit (SISo)i
a___
F (1?p) ?
(6)
Analysis of the Errors Made in the Calibration of Film Dosimeters. The random errors and the syste-
matic error-made in the measurements with a calorimeter do not exceed 0.1%. When the flux density of the en-
ergy of an electron beam is measured, additional systematic errors arise. A portion of the energy of the elec-
tron radiation is carried away by bremsstrahlung and is not recorded by the calorimeter. The error which is
made for this reason at an electron energy of 300 keV does not exceed 0.1%. The error which results from the
energy fraction carried away by electron backscattering does not exceed 0.3%. The error which is associated
with the measurement of the cross section of the beam of electrons incident upon the calorimeter is less than
0.3%. The error which results from a possible deviation of the calorimeter axis from the axis of the electron
beam does not exceed 0.6%. The error resulting from electrons scattered in the collimator does not exceed
0.570. Thus, the total error which is made when the calorimeter is used to measure the density of the energy
flux of the electron radiation does not exceed ?1% at the 0.95 confidence level. The coefficient k of Eq. (1),
which relates the calorimeter readings and the monitor readings, is obtained from several measurements. For
six measurements the error made in the determination of k amounts to ?2% and originates from fluctuations of
both the flux density and the electron energy. When the set of films is irradiated, a space charge accumulates,
and this may increase the backscattering of the electrons. In order to reduce a possible influence of this ef-
fect, the sets of films were wrapped in 10-i.-thick aluminum foil which was grounded. The error resulting from
the uncertainty of the coefficient of electron backscattering from the set of film detectors does not exceed 3%.
Thus, when the film dosimeters are calibrated, the energy transfer and the energy absorbed by the set are de-
termined with errors of ?2.3 and ?4%, respectively.
The experimental data were processed on a Mir-1 computer with the least-square method; the optimal
degree of the approximating polynomial was determined with the Fischer criterion [8],
Experimental Results. Chemical film dosimeters made from cellophane to which thiocyne red had been
added (prepared in the L. V. Pisarzhevskii Institute of Physical Chemistry, Academy of Sciences of the Ukrain-
ian SSR) were calibrated on the EOL accelerator. The initial electron energy was 360 keV and the accelerator
current ranged from 0.5 to 10 mA. The films were irradiated at a distance of 13 cm from the exit window of
the accelerator. The average energy of the incident electrons is 245 ? 15 keV, according to the calculation of
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[9], which takes into consideration the absorption of energy by both the foil of the exit window of the accelera-
tor and the air layer. The average energy of the incident electrons was determined as 235 ? 10 keV with the
aid of the calorimeter?collector. Within the experimental error limits, this value coincides with the calcula-
tions. The maximum rate of the dose absorbed by the films amounted to 1.2 Mrd/sec with these parameters
of the accelerator. The calibration curves obtained when the films were irradiated in fields of y radiation and
electron radiation are shown in Fig. 2. The films were calibrated in a photon radiation field with the aid of the
calorimeter apparatus described in [10].
The calorimetric apparatus and our method therefore make it possible to calibrate various film dosi-
meters with proper regard for the nonlinear relationship between the optical density (or any other parameter)
and the absorbed dose at electron energies of 0.15-2.5 Mev and at energy flux densities of 10-3-10 W/cm2. An
analysis of the errors of the calibration method, of the random error, and of the systematic error of the opti-
cal density measurements performed on the film has shown that cellophane films can be used to measure ab-
sorbed doses of electron radiation with an error of ?(15-20%). The apparatus was certified as a measurement
standard of the first-class category.
LITERATURE CITED
1. 0. B. Evdokimov and N. P. Tubalov, in: Dosimetry and Radiation Processes in Dosimetric Systems [in
Russian], Fan, Tashkent (1972), p. 52.
2. W. McLauglin, in: Proceedings of the IAEA Symposium ? Large Radiation Sources for Industrial Pro-
cesses, Vienna (1969), p. 579.
3. H. Eisen, "Electron depth-dose distribution measurement in metals and two-layer slabs," Doctorial Dis-
sertation, Univ. of Maryland (1971).
4. J. Puig, in: Proceedings of the IAEA Symposium ? Colloque sur la Radiosterillsation des Produits Medi-
caux et des Tissus Biologiques, Bombay, Dec. 9-13, 1974, SM-129/18.
5. B. Radak, in: Proceedings of the IAEA Symposium ? Dosimetric Techniques as Applied to Agriculture,
Industry, Biology, and Medicine, Vienna, April 17-21, 1971, SM-160/31.
6. A. K. Dmitriev et al., in: Dosimetry and Radiation Processes in Dosimetric Systems [in Russian], Fan,
Tashkent, (1972), p. 57.
7. V. F. Baranov, Dosimetry of Electron Radiation [in Russian], Atomizdat, Moscow (1974).
8. S. Brand, Statistical Methods in the Analysis of Observations [Russian translation], Mir, Moscow (1975).
9. M. Berger and S. Seltzer, Studies in the Penetration of Charged Particles in Matter, Washington, D. C.
(1964).
10. V. A. Berlyaed, V. V. Generalova, and M. N. Gurskii, At. Energ., 38, No. 4, 253 (1975).
221
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DE POSITED PAPE RS
SPATIAL DISTRIBUTION OF d?d NEUTRONS
D. V. Viktorov and T. S. Tsulaya
UDC 539.107.48+521.039
A study has been made of the spatial distribution of neutrons from D(d, n)3He in relation to angle of emis-
sion.
The specific fluence f from a circular target (radius R) at point (/ cos a, / Bina, L) in space is repre-
sented as
where
and the dimensionless symbols are
(y, 1, a, L)= (112a0R2) (10+ ail F a212),
zn
10= (0, ;
2n dx do)
PS
O o
2s1
I=?SS
xax K (ft, e) cog() ,
po
O o
2n1
12 -= K(0) cosi? x dx26)
- Po
O 0
r Rx; p=Rpo; 1= Rio; L =RLo.
(1)
(2)
(3)
Here ao is a normalization vector, p is the distance from a point on the target (rcosw, r since, 0) to the exposure
point, r and co are polar coordinates in the target plane, while the parallel deuteron beam incident on the target
lies in the oxz plane and at an angle y to the ox axis, and if and Oare the angles of incidence of the deuterons in the
laboratory system and in the center-of-mass system, respectively [I]:
cos0=? (i cos a cos y L sin y? r cosy cos (o);
p2 = r2 + /2 ?2r/ cos (c)? a) +L2;
cos 0= ?5 sin2 0+ cos 0 "V-1 ?62 sin2 ;
K ( d cos 0
?' =?
e :6::s 0+ 1 ?52 (1-2 cos2 0)
V 1 ?62 sin20
../m3H (4)
cos (I.
62_
+2QIE
mja and m3He are the masses of a neutron and 3He, E is the kinetic energy of the deuteron in the laboratory
system, and Q is the energy released in the reaction.
Series expansion in terms of the small parameter 6 provides formulas for the specific flux of (1) with a
computational error not exceeding 0.1%.
A program has been written in the "Engineer" autocode and a series of calculations have been performed
with a Minsk-2 computer; the dependence of f on the parameters y, 4 a, and L is presented for the case E =
0.206 MeV (al = 1.27; a2 = 0.26 [2]) and R = 0.7 cm via graphs, which show marked anisotropy.
The theory is compared with experiment in terms of the specific fluence averaged over the volume of the
detector:
(5)
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 203-206, March 1977.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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The observed Twere determined by an activation method at a small distance from the target in the neu-
tron generator; the reactions were 111Cd(n, n'), 111mCd and 31P(n, p)31Si, and the deuterons accelerated to 0.180
MeV fell on the target at y = 35?. The detectors (cadmium foil and plastic scintillators containing dispersed
calcium phosphate) were coaxial with the target and parallel to the plane of the latter; the neutron energy was
2.76 MeV. The neutron source in the first reaction was a standard titanium target, while in the second case it
was packed copper wool.
The measured rwere in reasonable agreement with the theoretical values.
LITERATURE CITED
1. L. I. Schiff, Quantum Mechanics, McGraw-Hill (1965).
2. J. Marion and J. L. Fowler, Fast Neutron Physics, Part 1, Wiley (1963).
(No.899/6906. Original article submitted January 20, 1976; complete text 0.65 authors' folios, 5 Figs., 3
Tables, 12 Refs.)
CALCULATIONS ON THE ENERGY DEPOSITED IN THE
SHIELD OF A FAST POWER REACTOR
V. A. Karpov, B. V. Koloskov, UDC 621.039.52
V. I. Matveev, and M. F. Troyanov
The shield of such a reactor has a complicated shape; e.g., the core in the BN-350 reactor was hexa-
gonal in the measurement period after the physical commissioning [1, 2]. A computational analysis is pre-
sented via the VIKAR and KENT two-dimensional program [3], which involves solving the diffusion equation
for hexagonal geometry, and it has been found that the differences in reaction rate, e.g., for fission of 235U, are
large in the high-enrichment zone with regard to directions at an angle in the wall and at the middle of the
wall, while in the first layers of the blanket (15-20 cm) the ratio of the fission rates at a given radius is about
2.
Table 1 compares the theoretical and observed fission rates for 235U and natural uranium observed dur-
ing the physical commissioning of the BN-350; the calculated distribution of the fission rate for 235U agrees
satisfactorily with the measured value (within 5 and 10% for the core and blanket, respectively, [1]). However,
the calculations for hexagonal geometry for natural uranium agree much better with experiment for the core
and blanket than do results for the one-dimensional case.
TABLE 1. Comparison of Observed and Calculated Fission Rates for 235U and Natural
Uranium (directed to a corner of the core)
R, cm
2 35IT
Natural uranium
19
8
c4
g
E-, g
z
b0
experiment*
g0.
, ,
?=0
b0
cinEi cr4
0.
z
experiment*
0
1
1
1
1
1
1
1
+29,5,
0,936
0,964
0,951-
0,957
0,969
0,979
1,02
0,920
0,938
0,967
0,?48
-29,5 T
0,936
0,948
0,936
0, 85
1,02
0,905
0,927
0,963
49,2
0,755
0,812
0,837
0,814
0,991
0,903
0,900
0,964
+59,0 t
0,662
0,693
0,712
0,624
0,675
0,672
0,679
0,945
0,850
0,879
0,831
0,784
0,878
-59,0
0,662
0,672
0,695
0,646
0,945
0,825
0,858
0,754
0,737
0,792
68,8
0,528
0,554
0,571
0,538
0,571
0,750
0,690
0,708
0,647
+88,5t
0,270
0,287
0,277
0,268
0,304
0,296
0,141
0,184
0,196
0,147
0,160
-88,5
0,270
0,279
0,271
0,285
0,141
0,178
0,191
0,181
108,2
0,083
0,094
0,090
0,082
0,081
0,097
0,095
0,029
0,031
0,030
0,034
0,039
0,036
-108,2 t
0,083
0,097
0,091
0,094
0,029
0,032
0,031
0,032
The different values for a single radius relate to different experiments, which differed in power level, irradia-
tion time, amount of detector material, etc.
tDistance reckoned in the opposite direction from the center of the reactor.
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Therefore, if the shape of the core in a fast reactor differs appreciably from a regular cylinder, the dis-
tributions of the various components responsible for the energy release, particularly fission of 238U, may vary
substantially with direction. In that case, it is necessary to perform calculations for hexagonal geometry, since
one-dimensional--models or two-dimensional cylindrical geometry can result in substantial errors in the energy
release in the blanket. The observed and theoretical distributions found for the BN-350 indicate that the VIKAR
and KENT programs give agreement with experiment, and the characteristics of the blanket can be determined
by means of a small number of groups (2-4). The same conclusion has been drawn elsewhere [3] for the core.
LITERATURE CITED
1. V. V. Orlov et al., At. Energ., 38, No. 2, 97 (1974).
2. A. Leipunski et al., Nuclear Power Plant BN-350, Sapp. to ANS-100, Detroit (1965), p. 15.
3. V. A. Karpov et al., At. Energ., 38, No. 4, 213 (1975).
(No. 896/8769. Original article submitted April 26, 1976; complete text 0.5 authors' folios, 1 Fig., 4 Tables,
7 Refs.)
THEORY OF NEUTRON-ACTIVATION MEASUREMENTS
IN BOREHOLES
G. S. Vozzhenikov and Yu. B. Davydov UDC 550.835
The distribution of the induced y radiation along the axis of a borehole of any radius has been determined
on the assumption that the material in the borehole differs in properties from the surrounding rock, in particu-
lar with regard to neutron and y-ray transport. It is assumed that the filling differs from the surrounding rock
in containing a uniformly distributed tracer, which is produced by nuclear reactions induced by thermal or fast
neutrons, the products producing y rays of a particular primary energy.
Certain restrictions have been imposed in solving this problem; it has been assumed that the angular dis-
tribution of the neutrons or y rays is isotropic and also that the energy losses in single elastic collisions are
small. This means that the multigroup diffusion approximation can be used, which simplifies the treatment
considerably.
Calculations have been performed on the flux of induced y rays due to the long-lived isotope of copper and
to 28A1 produced by 83Cu(n, y)64Cu; 28Si(n, p)28A1 by thermal and fast neutrons respectively; the independent
variable is the radius of the flooded borehole, the parameter of the curves being the distance from the activa-
tion point, and the calculations being for copper-bearing sulfide ores of various grades differing in density
and water content.
The following conclusions are drawn. The flux of y rays from the 64Cu at first increases with the radius,
but then decreases; the local peak is due to competition between processes. On the one hand, the flux due to the
rapid fast-neutron moderation in the water increases substantially, and such thermal neutrons activate the cop-
per. On the other hand, the induced y-ray flux itself is absorbed in the borehole. If the diameter is small, the
increasing flux of thermal neutrons predominates, but at large diameters the y-ray absorption becomes pre-
dominant. The induced activity in quartzite decreases monotonically as the borehole radius increases. The
fall in the activity is due to the rapid moderation of the fast neutrons and absorption of the induced y rays from
28A1 in the flooded borehole.
Figure 1 shows the induced 84Cu and 28A1 activities for a central probe; the activation medium was cop-
per-bearing sulfide ore and quartz sand of thickness such that the y-radiation flux tended to a limit, as did the
neutron moderation. The induced activity was recorded with a universal scintillation counter in conjunction
with an AI-128 multichannel analyzer. Good agreement was obtained between the observed and calculated func-
tions cp (h), where h is the thickness of the layer of water between the borehole wall and the body of the probe.
The function (I)(h) for thermal neutrons differs considerably from that for fast ones, as has previously been ob-
served by Vozzhenikov (in: Proceedings of the Sverdlovsk Mining Institute, Aspects of Prospecting Geophysics,
Issue 41 [in Russian], Sverdl. Knizh. Izv. (1962)). The peak observed as a function of borehole diameter for
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Quo
P(0)
100
50
0 10 h, cm
Fig. 1. Comparison of calcula-
tions and experiment for in-
duced activity of: 1) 28AI; 2) 84Cu
for a probe placed centrally in a
flooded borehole.
the (n, y) reaction (84Cu) and the marked fall in 28Si(n, p)28A1 as h increases would appear to indicate that it is
essential to consider the rock porosity in interpreting neutron-activation measurements in boreholes.
(No. 897/8830. Original article submitted June 8, 1976; complete text 0.65 authors, folios, 3 Figs., 4 Refs.).
THE DOSE DISTRIBUTION FOR A THIN NEUTRON BEAM
IN A TISSUE-EQUIVALENT MEDIUM
N. S. Budnikov and D. B. Pozdnee v UDC 577.3:539.12.04+539.125.52
A study has been made of the dose distribution in a tissue-equivalent phantom simulating muscle, the
beam being provided by a point unidirectional source (thin beam) for primary energies of 14, 10, 7, 5, 3, 1, and
0.1 MeV.
The first-collision dose has been calculated analytically, while the doses from the second and all subse-
quent collisions have been calculated by Monte Carlo methods. The latter have also been used to calculate the
transport of the resulting photons through the phantoms.
The details of the dose distribution are explicable in terms of the interactions between the neutrons and
the material in the phantom.
(No. 900/8771. Original article submitted April 30, 1976; complete text 1.1 authors' folios, 1 Fig., 30 Refs.).
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EFFECTS OF ANNEALING ON THE PROPERTIES OF
WELDED JOINTS BETWEEN URANIUM AND
ZIRCONIUM OR TITANIUM ALLOYS
V. R. Tatarinov, V. P. Ashikhmin,
and V. S. Krasnorutskii
UDC 621.791.762.1:(669.822
+669.295)-F(669.822+666.296.)
Measurements have been made on the mechanical parameters and structure of joints made by resistance
welding for rods of diameter 6.5 mm between uranium and titanium or zirconium, which have been examined in
the initial state and after annealing for various periods at temperatures between 450 and 600?C. Tests were
made on welds between uranium (99.8% purity) and technically pure titanium grade BT1-00s, and also with low-
alloy titanium (Ti + 2.2% Al + 2.5% Zr) and zirconium (Zr + up to 9.5% Cu + up to 0.5%Mo). Annealing reduces
the strength and plasticity. The rate of softening increases with the annealing temperature, and the fall in
strength or plasticity tends to a certain limit characteristic of each metal pair. For instance, joints between
uranium and BT1-00s gave tensile strengths reduced after 2000 h of annealing at 550?C from 44-107 to 25.5.i9
N/m2, with no further change.
Metallography showed that the changes in properties in welded joints of uranium?titanium and uranium?
zirconium types due to annealing are the result of the formation and growth of transitional zones, which con-
tain the intermetallides U2Ti and UZr2 as solid solutions. The densities of these deposits of distinct inter-
metallide phase increase continuously until a continuous layer of the intermetallide is formed, which appears
to represent an obstacle to further expansion of the diffusion zone.
Metallographic examination of fractures in welded joints after prolonged annealing shows that the failure
occurs along films of intermetallide, which thereby determine the mechanical characteristics of the joints af-
ter prolonged annealing at 500-600?C.
(No. 901/8792. Original article submitted May 10, 1976; complete text 0.5 authors, folios, 5 Figs., 2 Tables,
2 Refs.).
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LETTERS TO THE EDITOR
ANISOTROPY OF DOSE SENSITIVITY IN SEMICONDUCTOR
DETECTORS OF VARYING CONSTRUCTION USED FOR
DOSIMETRY OF IONIZING RADIATION
V. A. Manchuk UDC 53.089.5:539.1.074
Semiconductor detectors of nuclear radiation with an elearon-hole junction possess a number of advan-
tages which are the reason for their promising use in the dosimetry of x-ray and y radiation [1-3]. One of the
most important parameters of a dosimeter that determines its field of application to a considerable extent is
the dependence of its sensitivity on the orientation of the detector axis with respect to the direction of propa-
gation of the radiation. The present work presents the results of a study of the dependence of dose sensitivity
on the angle of incidence of x-ray and y radiation for several types of semiconductor detectors operating in
the short-circuit current measurement mode.
In dosimetric practice, it is often necessary to make measurements in fields of scattered radiation where
it is not possible to pick out a predominant direction of propagation for the quanta and to orient the sensor of
the detector in the best manner with respect to this direction. Hence the attempt of experimenters to produce
a dosimeter with minimal anisotropy of its readings is understandable. This parameter depends on a number
of factors, and primarily on the type of detector, the shape of its sensitive region, and the structural features
of the detector and its packaging. The ideal geometric shape of a detector is a sphere, but the manufacture of
semiconductor detectors with a spherical (or globular) sensitive region is an extremely difficult technical prob-
lem.
This paper describes test results for several laboratory and commercial models of semiconductor detec-
tors of varying construction. One of them was a surface-barrier silicon detector with a sensitive surface in
the form of a hemisphere 2 mm in diameter joined to a cylinder 3 mm high. The technology of its preparation
is given in [4]. A second sensor was made of two gold?silicon detectors of planar construction connected in
parallel with the sensitive surfaces facing in opposite directions. Detectors 4 x 8 x 1 mm in size were manu-
factured from silicon with a specific resistance of 6 ? 103Q-cm. The choice of such a system was dictated by
consideration of the comparative simplicity of its manufacture. Commercial models of semiconductor detec-
tors were tested in addition to the specified detectors prepared under laboratory conditions. There are well-
/ 2 3
Sensitivity, nA -min ?R-1
Fig. 1. Dependence of dose sensitivity of
a spherocylindrical detector on angle be-
t veen beam direction and detector axis.
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 207-208, March, 1977. Original article sub-
mitted September 15, 1975.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
227
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42 44 46 48 1,0
Sensitivity, nik ?min ?R-1
Fig. 2. Spatial characteristic of spherocylin-
drical detector measured after compensation
for "energy dependence:" 6.) 27 keV; A) 1250
keV.
known attempts of a number of investigators [5, 6] to use detectors of commercial manufacture in the dosi-
metry of x-ray and y radiation, the main purpose of which was radiometric and spectrometric measurements
[7]. However, the spatial properties of such detecors were not discussed.
In the present work, type DDS-5/2A diffusion-drift silicon detectors with a sensitive region 5 mm in
diameter and 2 mm thickwere tested. The ratio of the dimensions of the sensitive region for such a detector
correspond to the requirement for isotopy to a greater degree than in the majority of other known commercial
modifications. In addition, for purposes of comparison, a detector model differing from the DDS-5/2A only in
the thickness of the sensitive region, which was 0.22 mm, was tested.
The specified detectors were placed in the field of a standardized beam of x-ray and y radiation. Mea-
surements of the short-circuit current generated by the radiation were made for various orientations of the
detector axis with respect to the direction of the beam and for photon energies of 0.03-1.25 MeV. The mea-
surements were used to construct curves for the dependence of the current, normalized to the exposure dose
rate, on the angle between the axis of the detector and the direction of the beam. The dependence obtained for
the spherocylindrical detector is shown in Fig. 1. As is clear from Fig. 1, the detector current varies with
photon energy, which is associated with the significant "energy response" characteristic of silicon detectors
with respect to the exposure dose. Compensation of the "energy response" to a value not more than +10-15%
was achieved by means of sample metal filters predominantly of lead and copper.
Definitive measurements made it possible to establish that the DDS-5/2A detector was isotropic with re-
spect to dose sensitivity within a solid angle of 1.7-rr while the analogous detector 0.22 mm thick was isotropic
only within the solid angle 0.6r. Radial anisotropy was strongly expressed in the composite detector. Thus, a
reduction in sensitivity by 40% of the maximum value was noted for photons with energies of 0.03-0.07 MeV.
The use of detectors with thicker sensitive regions in combination with special filters made it possible to re-
duce the anisotropy. The spherocylindrical detector has the best spatial properties. As shown in Fig. 2, the
dose sensitivity falls within the limits 0.8-1.0 nA ?min ? 11-1 within the angle 0-0.757. Taking the axial sym-
metry of the detector into consideration, this means the isotropy of its sensistivity covers a solid angle of 3.3r.
Thus, data were obtained for the spatial properties of DDS-5/2A detectors that will make it possible to
make a sounder choice of these detectors in the future for specific dosimetric studies. The measurements per-
formed demonstrated the comparatively good isotropy of a spherocylindrical detector which, together with high
spatial resolution, furnishes the prerequisites for its application to the solution of abroad group of problems in the
dosimetry of x-ray and y radiation, including measurements in fields with a high dose-rate gradient characterized
by a significant contribution from scattered radiation or created by a set of distributed sources.
LITERATURE CITED
1. A. N. Krongauz et al., Semiconductor Detectors in the Dosimetry of Ionizing Radiation [in Russian],
Atomizdat, Moscow (1973).
2. R. Parker and B. Morlye, in: Proceedings of the IAEA Symposium ? Solid State and Chemical Radiation
Dosimetry in Medicine and Biology, Vienna, Oct. 3-7, p. 167.
3. A. A. Petushkov and V. A. Manchuk, Med. Radiol., No. 11, 52 (1971).
4. A. A. Petushkov, V. A. Manchuk, and Yu. F. Pryakhin, Prib. Tekh. Eksp., No. 1, 51 (1975).
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5. E. L. Stolyarova, S. N. Volodin, and V. V. Samerov, Vopr. Dosim. Zashch., No. 11, 168 (1970)?
6. Yu. M. Larioshin et al., Med . Radiol., No. 10, 70 (1971).
7. R. S. Reznikov and Yu. P. Sel'dyakov, Commercial Semiconductor Detectors [in Russian], Atomizdat,
Moscow (1975).
DISPERSIVENESS OF RADIOACTIVE AEROSOLS AT
THE NOVOVORONEZH NUCLEAR POWER STATION
S. S. Chernyi, V. P. Grigorov, UDC 621.039.58:541.182.2
V. I. Stepchenkov, and V. N. Kirichenko
Information about the dispersiveness of aerosols is required for rational organization of an air-cleaning
system and for ensuring representative sampling of the aerosols. Unfortunately, there is practically no infor-
mation about the dispersiveness of aerosols at nuclear power stations. In this paper, a study is made of the
dispersiveness of radioactive aerosols in the main ventilation systems of the third and fourth units at the Novo-
voronezh Nuclear Power Station (Table 1).
A six-cascade impactor (sixth cascade is an AFA-RMP filter) was used as a measuring instrument. The
backings of the impactor were covered by a thin layer of AFA-B filter (Petryanov tissue of mass 10-20 mg).
The efficiency for "adhesion" of aerosol particles to such backings is satisfactorily high [1]. The flow rate of
air passing through the impactor was 10 liters/min. Samples were collected over a period of 5-6 days; the
activity of aerosol particles collected on the backings was determined by means of standard radiometric equip-
ment after a holding time of 1 day.
It is well known that the size distribution of particle activity is most often described by the log-normal -
distribution
- 1(10-1g Sg)2
V gE ig ag exp[
2 1g2 Crg
(1)
where 0 is the diameter of an aerosol particle; 6g is the average geometric diameter of the particle; og is the
rms deviation of logd from log 6g. The log-normal distribution is completely determined by the parameters 6g
and crg. The determination of these parameters was also a purpose of this study.
The method described in detail in [2] was used to analyze the results. An impactor separates aerosol
particles into separate dispersive fractions in accordance with their aerodynamic diameters.
The aerodynamic diameter da of the particles is determined by the condition
Po6t=" P62, (2)
where p is the density of the particle material, g/cm3; Po is unit density, which is 1 g/cm3.
Results of the studies of radioactive aerosols in ventilation systems (see Table 1) showed that the dis-
tribution of particle mass and activity with respect to aerodynamic size is rather well described by a log-nor-
mal law. The averaged parameters for the distributions are given in Table 2 along with values for mean mass
concentrations. The parameters of the distributions of particle mass and activity with a respect to size do not
agree, which is evidence of the association of radioactive materials with fractions of a given dispersiveness.
The change in the ratio of relative activity of individual dispersive fractions of aerosols with sample
holding time after collection is of interest.
An analysis of the data obtained indicates that a constant ratio between the activities of individual
dispersive aerosol fractions is established after a sample holding time of 5 h. It is also clear that a
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 208-209, March, 1977. Original article sub-
mitted March 9, 1976; revision submitted November 3, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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TABLE 1. Main Ventilation Systems of
Units and Sampling Points
Ventilation
system
Stack
B-1
4B-2
4B-4
Aerosol
Purpose filters
present
ischarge of air
to theatmosphe
Ventilation of cen
tral hall for units
III and IV
Ventilation of
sealed, unserviced
areas of unit IV
Ventilation of
semiserviced
areas of technical
equipment in
units III and IV
entilation of
electric motors-
of main circulating
pump and main
restricted areas of
unit IV
I No
Sampling
points
Collector
Yes Before
aerosol
litters
TABLE 2. Aerosol Distribution with Respect
to Aerodynamic Size
Ventilation
system
Parameters of log-normal mean
distribution mass
particle particle concn.
activity
mass mg /cm'
8ag aa g aa g, a a g
Stack
4E1-2
121-3
4B-4
3,9 2,0 0,5 3,5 0,042
3,8 2,3 1,1 2,3 0,086
1,4 2,3 1,0 3,0 0,017
1,2 2,2 1,0 1,9 0,048
0,9 2,6 0,9 2,9 0,069
*Samples were collected over a period of 10 days
for the determination of the parameters of the par-
ticle mass distribution with respect to size.
significant portion of the short-lived radionuclides with half-lives less than 1 h is associated with aerosol
particles having a diameter less than 1 p. A similar pattern is also observed in the 4B-4 system. For the
other ventilations systems studied, this phenomenon is observed to an extremely insignificant extent and
changes do not occur in the ratios between the activities of individual dispersive aerosol fractions.
The authors thank M. A. Baranov, V. I. Kazakov, and S. M. Pankova for help rendered during the study.
LITERATURE CITED
1. A. A. Rusanov and S. S. Yankovskii, in: Impactors for Determination of Dispersyeness of Industrial Dusts'
[in Russian], Ser. Commercial and Sanitary Purification of Gases, Izd. TsNIITENeftekhim, Moscow
(1970), p. 30.
2. 0. M. Zaraev, B. N. Rakhmanov, in: Scientific Papers of the Institutes for the Protection of Labor [in
-
Russian], No. 71, VTsSPS, Profizdat, Moscow (1971), p. 53.
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TITANIUM ALLOYS AS STRUCTURAL MATERIALS
FOR LIQUID METAL RADIATION LOOPS
D. M. Z akharov UDC 669.295.018:669.87
The successful development of radiation loops requires investigations of the resistance of structural
materials in liquid metal y carriers. Titanium alloys are prospective structural materials. The resistance
of the titanium alloys VT1-1, VT-6, and VT-14 in liquid indium and in an indium?gallium alloy of 20.5 wt.%
indium at 350?C were studied in [1, 2]. Corrosion rates were measured in static tests which lasted 400 h or
less.
In the present paper we report on a continuation of the previous studies: corrosion rates are measured
in prolonged static tests of samples at 350 and 420?C, and the effect of atmospheric oxygen on the corrosion
rate is estimated.
The passivation and testing procedures, data on the materials used, the chemical analysis etc. are given
in [1,2].
The corrosion rate is calculated from the equation
K =0.1 (Vptc)I (Sp2t),
where K is the corrosion rate in mm/h, pi and p2 are, respectively, the densities of the liquid metal medium
and the solute in wcm3, c is the concentration of the solute in wt.%, and t is the duration of the test in hours.
The parameter V/S is the ratio of the volume of the liquid metal medium to the surface of the sample. The ex-
perimental data obtained are listed in Table 1 which shows for comparison the results of [1] for short tests.
In all cases the system consisting of structural material and liquid metal medium was not evacuated. The
following conclusions can be drawn from Table 1.
1. The corrosion rate of titanium alloys in liquid indium is practically independent of passivation. Under
identical temperature conditions the corrosion rates of various titanium alloys are nearly the same. As the
length of the test is increased the concentration of titanium CTi in liquid indium increases insignificantly, and
the corrosion rate of titanium alloys tends to decrease. The corrosion rate is not increased when the tem-
perature of the test is raised to 420?C.
2. At 350?C in the indium?gallium alloy medium the corrosion rate K of passivated titanium VT1-1 is 25
times lower than that of a nonpassivated sample. This results from the protective effect of the TiO2 oxide film
which, however, develops only in the short tests (400 h). Under the prolonged action of the indium?gallium al-
loy (up to 1000 h and more) the oxide film is destroyed and the corrosion rate is increased appreciably.
3. Pass ivation does not have an appreciable effect on the solubility of the VT-6 and VT-14 titanium alloys
in the indium?gallium medium. This may be due to the low oxidizability of the alloyed titanium and to other
causes [1, 21.
Increasing the duration of the test of the VT-6 and VT-14 samples to 1000 h has practically no effect on
the titanium content in the indium?gallium alloy.
4. The solubility of titanium alLoys in the indium?gallium medium is higher than in indium, but in all the
cases examined the titanium content is considerably below the maximum solubility at the corresponding tem-
peratures [2].
In order to estimate the effect of atmospheric oxygen on the corrosion rate of titanium alloys, tests were
performed on passivated and nonpassivated VT1-1 and VT-14 samples in special samples at a residual pressure
of 5.10-3 mm Hg. The results of the tests are shown in Table 2.
Translated from Atomnaya gnergiya, Vol. 42, No. 3, pp. 210-212, March, 1977. Original article sub-
mitted April 12, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
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TABLE 1. Concentration of Titanium in Indium and in Indium-Gallium Alloy, and Cor-
rosion Rate of Titanium Alloys
Liquid
metal
medium
Nonpassivated- sample -
Passivated sample ?
Dura-
ti.011 Of
test,
VT-I; V/S=2
VT-6; V/S=4
VT-14; V/S= 4
VT-1; V/S=2
VT-6; yis=4
VT-14; V/q=4
'
350
420
350 I
420
350- 420
_ 350 '420
350
420
350 I
420
h
.c
Indium-
gallium
alloy
0,8*
-
-
0,43
6,0
0,8
-
-
0,38,
-
0,03
0,21
0,3 .
0,84
-
-
0,38
5,3
0,94
-
-
?
0,29
-
-
40011)
l"
.
5,6
0,7
1,94
5,3
0,4-
0,21
4,47
2,24
5,2
1,22
Inditun
0,0670,03
_
-
.0,15
-
0,24
0,45
0,014
_
0,23
0,026 '
?
-
0,1
0;1
0 015-
,
.
- ,
-
0,1.6
?0,3 .
0 028
, .
-
-
.0;16
.59.1.1)
1900
3500
4,4
0,13 .
_
?3,8
0,07
1,8
'
0,093
1,7
0,1
0,32 :
0,1
0,1 -
1,9
-
0,17
3,7'
0,14
?0;26
0,42
0,17
0,16
0,45
0,1
0,6 -
0,18
0,14
0,19
0,33
0,43
0,31
, 0,3
Here and in Table 2 the numerator is On ? 102 wt.%, and the denominator is K '106mm
TABLE 2. Titanium Concentration and Cor-
rosion Rate of Titanium Alloys in Indium and
in an Indium-Gallium Alloy in Vacuum Tests
at 350?C
Liquid metal
Nonpassivated
sample
Passivated sam
medium
VT-1; VT-14;
VTI-l;
VT-14;
V/S = 2 V/S = 4
Iris- 2
V/S = 4
Indium-gal-
lium alloy
0,05
0,1
0,026
0,06
0,14
0,56
0,073
0,35
Indium
0,026
0,075
0,03
0,075
0,025
0,14
0,03
0,14
tion of
test, ?
h
1000
3500
In evacuated and unevacuated ampuls the corrosion rate of titanium alloys in prolonged tests does not de-
pendon passivation (Tables 1 and 2), but is appreciably lower in evacuated ampuls. This effect of atmospheric
oxygen can be accounted for by thermodynamic considerations. According to data in [3], over a wide range of
temperatures titanium has an appreciably larger affinity for oxygen than do gallium and indium, since the
change in the Gibbs free energy in the formation of TiO2 (rutile) is much smaller than in the formation of Ca203
and In203, the most stable gallium and indium oxides. Therefore, the titanium in liquid indium and in the in-
dium-gallium alloy is able, under certain conditions, to attach the dissolved oxygen. Thus, in unevacuated
ampuls at a high temperature an oxide film is formed on the surface of the indium and the indium-gallium al-
loy, and simultaneously oxygen is dissolved in the liquid metal. Under these conditions various processes can
develop which lead to the formation of Ti02: the intense reduction of gallium and indium oxides by dissolved
titanium, the interaction of dissolved titanium with dissolvedoxygen, etc., which ultimately decreases the con-
centration of dissolved titanium in the liquid metal medium and thus stimulates the further solution of titanium
alloys with an increase in the total titanium content (dissolved titanium and combined titanium ofthe dioxide)in
the melt.
In the evacuated ampuls, these processes for forming TiO2 are weaker, and therefore the titanium concen-
tration is lower.
It should be noted that in testing the titanium samples a characteristic grayish-bronze film is formed on
the surface of the indium and the indium-gallium alloy only in the unevacuated ampuls. The x-ray structural
analysis of the film indicates that it is complex in composition, and definitely establishes the presence of the
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TiO2 phase with the rutile structure, which agrees with the reasons stated for the intense oxidation of titanium
in liquid indium and the indium ?gallium alloy in unevacuated samples. The presence of TiO2 in the surface
film is explained by the low density of Ti02.
From experience with the construction and use of radiation loops it is known that under strictly equivalent
conditions an indium?gallium alloy is more fluid when circulating in titanium pipelines than in 110118N9T
stainless steel pipelines. This results from the fact that over a wide range of temperatures the change in the
Gibbs free energy is larger in the formation of Fe203 than in the formation of the oxides Ga203 and In203 [3],
and therefore in stainless-steel pipelines gallium and indium will be oxidized as a result of the reduction of the
Fe203 film which is always present on a steel surface. It is known [4] that gallium and indium oxides are easily
wetted by an indium?gallium alloy, and therefore with an increase in the oxide content a pasty viscous mass
composed of oxides and alloy appears, greatly impairing the fluidity of the y carrier. On the contrary, tita-
nium can reduce the gallium and indium oxides contained in the liquid metal; i.e., in titanium pipelines an
indium?gallium alloy will be cleansed of gallium and indium oxides which are present or produced.
Thus, titanium alloys have very diverse favorable properties as structural materials for radiation loops.
The negligible dissolving of titanium alloys does not give rise to problems of the contamination of the ycarrier.
An important role is played by the decrease in oxide content of a y carrier circulating in titanium pipelines,
and this contributes to an increase in fluidity. Here it should be stated that there are serious doubts about the
expediency of preliminary passivation of titanium alloys, in particular, the VT1-1 alloy used in radiation
piping. First of all passivation is effective only for a short contact with y carriers, and secondly the presence
of a passivating film has the undesirable effect of lowering the ability of titanium to reduce gallium and indium
oxides.
The authors thank S. P. Yatsenko for all-around assistance, and Z. P. Danelyan for help with the experi-
ments.
LITERATURE CITED
1. D. M. Zalcharov et al., At. Energ., 35, No. 3, 202 (1973).
2. S. P. Yatsenko et al., Fiz.-Khim. Mekh. Mat., 10, No. 2, 51 (1974).
3. U. D. Peryatin, V. P. Mashirev, and N. G. Ryabtsev, Thermodynamic Properties of Inorganic Materials
[in Russian], Atomizdat, Moscow (1965).
4. D. M. Zakharov, At. Energ., 39, No. 4, 290 (1975).
USE OF PERTURBATION THEORY FOR EXPERIMENTAL
STUDY WITH A PULSED NEUTRON SOURCE
V. Ya. Pupko, V. A. Tarasov, UDC 621.039.519.4
and A . K. Sharapov
Along with the extensive use of perturbation theory for the effective neutron multiplication coefficient
(Ireff), perturbation theory for the eigenvalue of the quasistationary transport equation for prompt neutrons,
? (WO c1)= ?la, V9)(1', E, S1)1+ ?(1)--1-10(P (1)
is extremely effective in connection with the development of pulsed methods for measurement of the neutron-
physics characteristics of systems.
The operators ? and (5 are of the well-known form where (5 characterizes neutron production. The real
eigenvalue of the equation of least modulus can be measured experimentally. It is the asymptotic damping
decrement for the density of prompt neutrons after injection of a neutron pulse into a system, where the density
of neutrons in the system decreases exponentially in time [1, 21.
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 212-214, March, 1977. Original article sub-
mitted April 30, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
233
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GOQGGOOGGG
GGQQVGOGGOO
GOGOOGGGG
OGGGGOGGGO
,GOGGOGG4GG
,floGGGGA?GOGOGG
et;OGOGOGOGGer
ftGGOGGOGGGG
tieGGGG@GGIGG
9..f.11)7Z/Zrlikatima,=,
-f,) ardi-rf -65 ti
X-370 nun ,.,
et-2
? ? 5
Fig. 1. Loading chart and arrangement of experi-
mental points; 1) group of nine cells for measure-
ment of perturbations in a subcritical reactor; 2)
measurement points for distributions in a critical
reactor; 3) detectors; 4) expanders- for measure-
ment of lateral leakage factors; 5) target of neu-
tron generator.
Perturbation theory for a, in contrast to perturbation theory for Reif, can be applied to multiplying and
nonmultiplying systems. With the aid of this theory, it is convenient to measure such parameters as lifetime
and generation times of prompt neutrons, the coupling between change in system composition and change
in system size, the average neutron diffusion coefficient, the cross section for a 1/v absorber, etc. It
was shown [2] that the solution of the nonstationary neutron transport equation can be obtained by ex-
panding its solution in terms of the eigenfunction of the quasistationary Eq. (1), which makes it pos-
sible to be able to find the solution of that equation. The constants and method of calculation for that equation
should, in principle, be determined in more accurate fashion from the results of studies of nonstationary neu-
tron flow; this is conveniently done by means of pulsed experiments. The perturbation theory for a yields a
system of functionals which can be used for this purpose.
The present work presents measurement results for several functionals, evaluates measurement accu-
racy as a function of the suberiticality of a system, and verifies the theoretical relations in perturbation theory.
Perturbation theory for a was described in [3, 4]; several problems of the experimental studies based on
it were described in [5, 61 and in the compilation [2]. It was found that for a variation of the medium constants
the variation of the decrement was
(c+ 820 + (a)+, 6-00
(V-, limp) 9
and for a geometrically similar variation in the dimensions of the system
SR f(p+ (0, Vq)))
R (cp+, 1 /Q) '
(2)
(3)
where R is a characteristic dimension of the system. Here, (p(r, E, is a solution of Eq. (1); (p+(r, E -SI) is a
solution of the adjoint equation and the parentheses denote integration over all variables.
We introduce some definitions [7]. The limit of the sum over the volume of the system of the perturba-
tion 6a resulting from the replacement of the material of density po ma volume av ? 0 by a void is n ? the
total effectiveness index for system index for system material with respect to a. From Eq. (2) we have
*po is the density of a mixture of different nuclei, the ratios between which are unchanged.
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TABLE 1. Results from Measurements of
Perturbations of the Damping Decrement
Quantity
determined
Reactor height, cm
27,0
19,2
12,8
Keff *
a, sec-1312+2
n, sec-1
(1i-ka)/3.sec-1
co, sec-1
T, ?sec
1, ?sec
( vDB2),cm-1
Measurpment
error, */0
1,0064
24850+300
8390+100
8380+100
29,3+0 .3 (30,3) *
29,1+0,3
12580+150
1-1,2
0,8654 0.6714
4050+40 8715+200
17850?10009950?2000
7300+300 6220+700
7540+200 5870+400
30,1?0,7 53,3?6,0
27,8+0,6 36,4+3,0
10950+500 9300+1000
2,5-5,6 10-20
*Calculated data taken from [5, 6].
&)]
1 p
= urn2 (Au) po
(9)+, 1/4) (4)
V
AV-.0
Assuming that shielding of the system material is small, the dependence on p in the numerator of Eq. (4) dis-
appears. In that case
ifT) + (cp+, 00 ? 139 (actiap)v.
(cp*, 1 / vg)
(4a)
The neutron leakage factor with respect to (2, is determined from the variation of the decrement for geo-
metrically similar variations in the dimensions of the system:
(0= ? lim Vo ?Va (0a1017),.
AV?.0
Vo is the original volume of the system. In the general case [7],
1 [*(Q, VW)]
= 3 (T*, 1//4) ?
Between r and w there is the relation
1
For poisoning of a system by a 1/v absorber, (51 = ?Pa(akTvklIv), hence we have from Eq. (3)
6c4=6PaakTvhT,
which makes it possible to determine the cross section of a 1/v absorber at the neutron energy kT.
With replacement of the fuel by an equivalent absorber (61 = 0, (5-( = Q) [4, 51, we have
urn -0(p)
(6a)e ? a ? (cr, livcp) ?
(5a)
(6)
(7)
(8)
Equation (8) makes it possible to determine the average prompt-neutron generation time T = (p+, 1/vcp)/
((p+ , 4.0. The ave ge prompt-neutron lifetime / = ((p+ , 1/v)/ [p, Vip)]?(p+, 1(p)can be determined from the
relation [1, 2]
a= (1//)? (1/T).
+ a = 3o.) = ?2(q, DV2q))/ (q)+,
ri a= 3(0= 2 (vD/32).
The averaging is performed with a weight ((p+ , 1/v(p).
The measurements were made in a heterogeneous uranium?water reactor without reflector in the shape
of a parallelepiped having fuel elements of highly enriched uranium 10 mm in diameter arranged with a 32-mm
In the diffusion approximation [4],
For a system without a reflector,
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spacing [5] (see Fig. 1). Subcriticality was varied by variations in the height of the reactor. The equipment
used and the method for determination of a were similar to those described earlier [2, 5, 6].
The results of the measurements are presented in Table 1. To determine the effectiveness index, we
measured the perturbation resulting from the replacement of the volume of an equivalent cell by a void with
subsequent summation over the volume of the reactor. The replacement was performed with consideration
given to the symmetry of the reactor with respect to a single cell in a critical reactor orwith respect to a
group of several cells in the subcritical state of the reactor (see Fig. 1). The leakage factor was measured
by sequential variation of the dimensions of the reactor along the three directions. In this case, co = (1/3)(cex +
cey + wz) for a parallelepiped assuming separation of variables, where cox," are the leakage factors along the
individual directions defined as cox = ?X(aa/ax)p for changes in the X dimension, etc. A measurement with re-
moval of a complete cell, i.e., fuel and moderator simultaneously, takes into account shielding of system ma-
terials within a cell in accordance with Eq. (4).
A mixture of boron and aluminum oxide powders was used as an equivalent absorber. The correction for
the discrepancy between the cross section of this material and that of the fuel, which is 0.035, was taken from
[5]. The reactor was poisoned with boric acid in both the critical and subcritical states. For boron, ukT
738 ? 20 b.
The experimental data confirms the theoretical relation (6). This fact opens up additional possibilities
for experimental studies, for example, to measure the total effectiveness index of the materials with respect
to changes in the size of the system. The results point to the possibility of measuring the functionals in the
perturbation theory for a and a number of neutron-physics parameters of systems at varying subcriticalities.
LITERATURE CITED
1. Proceedings of the IAEA Symposium ? Pulsed Neutron Research, Karlsruhe, May1-14,1965, Vols. land
2. V. V. Orlov and t. A. Stumbura (editors), in: Theoretical and Experimental Problems of Nonstationary
Neutron Transport [in Russian], Atomizdat, Moscow (1972).
3. E. Pendlebury, Proc. Phys. Soc., A68, 474 (1955).
4. V. Ya. Pupko, Preprint FEI-103, Obninsk (1968).
5. B. I. Kolosov et al., At. Energ., 32, 579 (1972).
6. E. A. Stumbur et al., in: Transactions of the Power Physics Institute [in Russian], V. A. Kuznetsov
(editor), Atomizdat, Moscow (1974), p. 138.
7. V. Ya. Pupko and R. M. Strutinskii, in: Transactions of the Power Physics Institute [in Russian], V. A.
Kuznetsov (editor), Atomizdat, Moscow (1974), p. 174.
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xr,Aiky SPECTROMETER WITH AN Si(Li) DETECTOR
M. Vidra UDC 535.853
In the usual charge-sensitive preamplifiers used to amplify signals from a semiconductor detector, a re-
sistance which connects the gate of the field-emission transistor (FET) and the output of the preamplifier is
used to set the dc mode at the input of the FET. In addition to Johnson noise (dun = 2kTKdf), however, this re-
sistance contributes an extra noise component which drops like 1/fawith increase in frequency. The cause of
this extra noise is the imperfect structure of the resistance.
A preamplifier has been described [1] in which the resistive feedback was replaced by an electro-optical
feedback. Preamplifier noise was significantly reduced because of elimination of the resistance in the gate cir-
cuit and through the reduction in distributed input capacities. Another form of nonresistive feed back was des-
cribed in [2]. To compensate for the detector current (i.e., inverse current and the current induced by re-
corded radiation), they used both the gate current of the FET and its dependence on the voltage between the
source and drain (the gate current rises exponentially as the voltage between these electrodes increases). The
noise does not exceed 100 eV in such preamplifiers using Si(Li) detectors with a sensitive surface having an
area of 12 mm2. When making measurements, quasi-Gaussian shaping of electrical signals was used with a
time constant of several tens of microseconds.
In the preamplifier of the spectrometer, drain feedback was used, which is somewhat simpler than the
electro-optical feedback andpermits the achievement of identical results. Electrical signals from the detector
(Fig. 1) were fed into the gate of the FET (type 2N/4416) and then into the input of the amplifier (A1). Feedback
of the ac component was accomplished through the capacity Cf = 0.15 nF. A signal was taken from the ouptut
of A1 for control of the drain?source voltage Ud_n. An integrator was used to eliminate oscillations in the
drain?source voltage control circuit.
With an increase in detector current, because of radiation for example, the average value of the Voltage at
the output of A1 rises and the Ud...n voltage is correspondingly increased. The rise in this voltage produces an
increase in the gate current of the FET. The reverse process occurs with a drop in detector current. In this
way, equilibrium between detector current and data current is ensured; the preamplifier is in an operating
state at all times. The rest of the spectrometer is constructed in the standard manner.
4
Fig. 1. Block diagram of the spectrometer; 1) detector supply; 2)
detector; 3) cooled portion of preamplifier with detector; 4) pre-
amplifier; 5) FET; 6) pulse-shaping amplifier; 7) multichannel
pulse-height analyzer; d) drain; s) source; g) gate.
Institute of Nuclear Research, Rzhezh, Czechoslovakia. Translated from Atomnaya Energiya, Vol. 42,
No. 3, pp. 214-215, March, 1977. Original article submitted May 10, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
237
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2.105
Channel
Fig. 2. 241Am? spectrum (pulse-shaping time, 9 ?sec , detec-
tor voltage, 300 V)?
Pulse
2103 generator
Channel
Fig. 3. 55Fe spectrum (pulse-shaping time,
14 ?sec, detector voltage, 300 V).
For radiation detection, an Si(Li) detector was used which had a sensitive region 5 mm in diameter and
a compression layer 3 mm thick. Like results were obtained with detectors manufactured in Czechoslova-
Ida and East Germany. The detector, together with the FET and elements of the feedback circuit, was placed
in a cryostat with a beryllium entrance window 200 pc thick.
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400
300
a 200
0
0 5 10 15 20
Energy, keV
Fig. 4. Energy dependence of spectrometer
energy resolution.
25
A portion of the radiation spectrum from 241Am is shown in Fig. 2 (energy region is ?=?? 11-60 keV). The
55Fe spectrum obtained with the use of this detector is shown in Fig. 3. An instrumental resolution of 169 eV
was obtained at 5.9 keV (Mn Ka line). An approximate dependence of energy resolution on radiation energy is
shown in Fig. 4 for pulse-shaping with a time constant of 8 ?sec.
LITERATURE CITED
1. F. Goulding et al., Nucl. Instrum. Methods, 71, 273 (1969).
2. E. Elad, Nucl. Sci., NS-19 No. 1, 403 (1972).
FLOW CHARACTERISTICS FOR HOT WATER AT AN
INITIAL PRESSURE OF 2 2.8 MPa ESCAPING INTO
THE ATMOSPHERE
D. A. Khlestkin, V. P. Kanishchev, UDC 621.039.58:621.311.25:530.91
and V. D. Keller
Analysis results for emergencies occurring through leakage in the first loop in a nuclear power station
are very much dependent on the values assumed for the water flow rate and the composition of the water?steam
mixture
Calculations on critical flow rate are currently based on trends derived from experimental systems;
measurements have been reported [1] for the specific critical flow rate for values of the initial parameters up
to the critical level (F = 647.15?K, p = 22.5 MPa). The results presented here represent an extension of earlier
measurements, and they refine the values for critical flow rate at temperatures near the saturation point, far
from the boiling point and at critical and supercritical initial parameters. The measurements were made with
equipment previously described [1]. The measurements were supplemented by means of a check thermocouple
to indicate the water temperature at the inlet; the tests involved isobaric increase in the water temperature at
the inlet. Each working condition was maintained until all the parameters had stabilized. The configuration
of the working parts was as before. Cylindrical pipes with sharp inlet edges were used, with diameters of 3.6
mm and a ratio lid of length to diameter of 0.5, 1,5, or 6.0. The flow factors for the working parts were deter-
mined for water at room temperature with an initial temperature of 3-4 MPa, which were measured?for L = //d
of 0.5, 1.5, and 6.0. Here Pip was 0.723, 0.683, and 0.61, respectively. The results were worked up in terms of
Translated from Atomnaya Lergiya, Vol. 42, No. 3, pp. 216-218, March, 1977. Original article sub-
mitted May 28, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N. Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50. ?
239
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240
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fre
Ag
45
42
45
144
45
47
49
;5 A
47 -
46 -
a
41
1 42 4Ia 414 45 c4I cl 1
7 48 49
Po
43 41 42 143 44 45 0,6 47 48 49 tO Po
Fig. 1. Relative specific flow rate on leakage to the atmosphere
as a function of initial pressure for L = 0.5, p h =0.723 (a); L =
1.5, ph = 0.683 (b); L = 6, ph = 0.61 (c).
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ire against /30, where jre = jex/jh? in which jex is the experimentally measured specific flow rate, while jh is
the specific hydraulic flow rate as determined from the equation jh = (Po -Pco)/v, where, pc, is the initial
water pressure, pce is the counterpressure, and v is the specific volume of water under the initial conditions;
/30 = Po/per, where per is the pressure at the critical point of water. Figure 1 shows the results as Ocr = To/Ter
(the relative initial temperature ahead of the working section), where Ter = 647.3?K is the critical point of wa-
te r.
The following are the reasons for using these relative coordinates; graphical representation indicates the
regions of metastable and equilibrium flows, while it is possible to compare the measurements for various
initial conditions, and also it is possible to define the flow rate more precisely for the most characteristic
state.
Figure 1 shows the relative maximal and critical specific flow rates for pipes having L = 0.5, 1.5, 6.0,
respectively; these curves are derived by smoothing numerous measurements, whose maximum coefficient of
variation was i5%. Curves BCK (parts a and b) and BK (part c) correspond to escape of water having the satu-
ration temperature at the inlet to the pipe. Lines CD i and GiEj (where i = 1, 2, ...) are isotherms. The fur-
ther an isotherm from the saturation line, the greater the deviation from the boiling point at the inlet for the
particular initial pressure-. The relations of L of 0.5 and 1.5 go with the result for L = 6 to reveal characteris-
tic features for the flow in short and relatively long pipes. These features have been observed in less pro-
nounced form previously [1, 2].
Parts a and b of Fig. 1 show that there are two clearly defined major zones. The zone above line BCD
represents substantially metastable flow, while DCK corresponds to a considerable reduction in the meta-
stability, and the flow approaches the equilibrium state as the critical point K is approached. The metastable-
flow region occurs only for only relatively low-temperature water in the case of L = 6.0, and there is no clear
boundary. The flow of water at its saturation point is close to equilibrium at almost all initial pressures. For
130 a' 0.85, the flow characteristics for water near its saturation point for short pipes are almost the same as
those for L = 6.0, because in this range the pressure along the spinodal liquid cannot exist. It has previously
been supposed [I] that a completely metastable flow occurs for 00 < 7.0 MPa, but this is inaccurate. More care-,
ful examination has shown that water having the saturation temperature does not pass through the pipe with
100% metastability in this range. Parts a and b of Fig. 1 show that the range BC lies about 15% below the
100% metastability line, which is theline parallel to the abscissa and starting from point A. Our experiments
did not produce completely metastable flows under all conditions. The refined flow characteristics for L=6
indicate that equilibrium flow occurs in this case for /30-- 0.62 MPa. For instance, it has been reported [3] that
the specific flow rate for saturated water is 2.69 kg/m2? sec for homogeneous equilibrium model at P0=14
MPa. The observed value for these conditions is in the range 2.67-3.0 kg/m2- sec.
Therefore, the extended and revised relationships for the specific flow rate should be used in conjunction
with the empirical curves reported previously [1].
LITERATURE C ITED
1. B. K. Mal'tsev, D. A. Khlestkin, and V. D. Keller, Teploenergetika, No. 6, p. 61 (1972).
2. V. S. Aleshin, Yu. A. Kalaida, and V. V. Fisenko, Abstracts for the Third All-Union Conference on Heat
Transfer and Hydraulic Resistance [in Russian], Leningrad (1967).
3. V. A. Zysin (editor), Boiling Adiabatic Flows [in Russian], Atomizdat, Moscow (1976).
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MEASUREMENT OF THE RATIO BETWEEN THE
CAPTURE AND FISSION CROSS SECTIONS
OF "9Pu
V. P. Bolotskii, M. V. Polozov, UDC 546.799.4:539.172.4.162.2
A.' N. Soldatov, and S. I. Sukhoruchkin
In order to find the ratio a between the capture and fission cross sections of 239Pu up to 30-keV energy,
this quantity has been repeatedly measured in the IBR-30 pulsed fast reactor [1, 2]. In this article we give the
final results of the measurements made by the group at the Institute of Theoretical and Experimental Physics
(ITgF). Control values of a obtained before 1972 were published in [2]. The data in [2] are not included in the
results of this present article (Tables 1 and 2).
In contrast with the measurements made at the ITEF up to 1970 [3], we increased the number of detectors
to eight, introduced separate registration of y quanta of different energies in order to allow for possible varia-
tions in the shapes of the y spectra, improved the energy resolution more than tenfold (16 nsec/m), obtained a
large number of independent exposures for statistical processing, and made the measurements with a specimen
with a much reduced impurity content of other isotopes.
The measurements were made on the 250-m time-of-flight base of the neutron spectrometer of the Labo-
ratory of Nuclear Physics of the Joint Institute for Nuclear Research (LNP JINR) with neutron bursts of about
4 ?sec. Fast fission neutrons and capture and fission y quanta were registered by detectors based on stilbene
crystals 7 x 7 cm in size with pulse-shape separator circuits [2]. The flux of incident neutrons was measured
by a battery of proportional counters containing enriched boron (SNMO-5). Shielding from neutrons scattered
by the specimen was effected by a layer of enriched boron (85% enriched, 2 cm thick), and low-energy y quanta
from the radioactive specimen were attenuated by a layer of lead 1 cm thick. For protection from yquanta and
TABLE 1. Results of Measurement of a for
239Pu
Ene rgy
range, keV
Specimen
i
0.64 g/cm2
thick
Specimen
1 g/cm2
thick
Mean from
measurement
-
made in -
1973-1974
0,1-0,2
0,88
0,94
0,93+0,13
0.2-0,3
0,89
0,93
0,92+0,08
0,3-0,4
1,21
1,16
1,17+0,08
0.4-0,5
0,53
0,60
0,59+0,04
0,5-0,6
0,66
0,76
0,75+0,11
0,6-0,7
1,58
1,43
1,46+0,18
0,7-0,8
0,94
1,01
1,00+0,10
0,8-0,9
0,74
0,79
0,78+0,11
0,9-1,0
0,77
0,76
0,76+0,12
1-2
0,82
0,85
0,85+0,07
2-3
0,97
0,97
0,97+0,11
3-4
0,77
0,66
0,68T-0,12
4-5
0,81
0,88
0,87+0,07
5-6
0,83
0,84
0,84;1:0,09
6--7
0,78
0,72
0,73T0,13
7--8
0,69
0,75
0,74-F0,07
8--9
0,56
0,56
0,56:F0,09
9--10
0,36
0,50
0,47-F0,10
10--15
0,44
0,49
0,48-F0,08
15--20
0,35
0,35
0.35+0,10
10--20
0,40
0,42
0,413+0,071
20--30
0,32
0,36
0,35+0,062
Translated from Atomnaya Energiya, Vol. 42, No. 3, pp. 218-221, March, 1977. Original article sub-
mitted June 7, 1976.
This material is protected by copyright registered in the name of Plenum Publishing Corporation, 227 West 17th Street, New York, N.Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying,
microfilming, recording or otherwise, without written permission of the publisher. A copy of this article is available from the publisher for $7.50.
242
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TABLE 2. Comparison of Results in [2, 3, 5] with Present Authors' Data
Energy range,
keV
Present
authors
[3]
[2]
[5]
Glain
[5]
Weston
[6]
0,1-0,2
0,93+0,13
0,88-F0,03
0,93-F0,14
0,87+0,015
0,871-F0,052
0,845+0,077
0,2-0,3
0,92-F0,08
1,07-F0,04
0,98T0,14
0,94-F0,010
0,927-F0,056
0,912-F0,094
0,3-0,4
1,17-F0,08
1,23-F0,05
1,15+0,16
1,16=F0,014
1,15-F0,069
1,15-F0,099
0,4-0,5
0,59T0,04
0,45=F0,05
0,62-F0,13
0,44+0,013
0,426T0,026
0,483-F0,058
0,5-0,6
0,75T0,11
0,75-F0,05
0,78-F0,13
0,72+0,040
0,718T-0,043
0,704-F0,069
0,6-0,7
1,46-F0,18
1,72+0,13
1,58T0,20
1,54-F0,040
1,488-F0,089
1,673-F0,133
0,7-0,8
1,00-T0,10
0,94-F0,09
1,02-F0,15
0,97-F0,017
0,890-F0,053
0.973-F0,087
0,8-0,9
0,78+0,15
0,78-F0,09
0,85-F0,13
0,82-F0,025
0,790=P0,047
0,778?0,101
0,9-1,0
0,76-F0,12
0,71H-0,08
0,93-F0,14
0,70-F0,026
0,675-F0,041
0,717+0,077
0,1--1,0
0,91T0,09
--
0,89
0,86
0,86
--
? 1 --2 ,
0,85-F0,07
1,02-F0,06
0,95-F0,14
0,84-F0,013
0,802?0,048
0,927-F0,093
2-3
0,97+0,11
1,23-F0,08
1,08-F0,15
1,00
0,972-F0,058
1,108?0,103
3-4
0,68-F0,12
0,967470,11
0,77
0,72-F0,066
0,738-F0,043
0,895-F0,086
4-5
0,87-F0,07
0,83-F0,10
0,84
0,87?0,040
0,8314:0,050
0,821T0,079
5-6
0,84-F0,09
--
0,81
0,82-F0,046
0,807-F0,048
0,867-F0,084*
6-7
0,73-F0,13
--
0,69
0,79-F0,040
0,745-F0,045
0,816-F0,086
7-8
0,74-F0,07
0,67-F0,07
0,73
0,64-F0,022
0,642-F0,038
0,629+0,073
8-9
0,56-F0,09
--
0,63
0,54-F0,022
0,5374-0,032
0,575+0,064
9-10
0,47-F0,10
--
0,65
0,55-F0,022
0,606+0,036
0,6171-0,067
1-10
0,748+0,048
0,82-F0,07
0,80
0,77
0,76
--
10 --20
0,413+0,071
--
--
0,48-F0,022
0,486?0,029
0,466-F0,05
20-30
0,350-F0,062
--
0,35-F0,018
0,332,E0,066
0,373+0,04
Note. In the second column, all the errors except for the range between 1 and 10 keV are statistical.
TABLE 3. Ratios of Variable Background
to Total Count in Radiation Channel (0.7
MeV