National Academy

Sciences National I Research Council

NUCLEAR

SCIENCE

SERIES

The

Radiochemistry

of Cesium

NUCLEAR

SCIENCE SERIES: MONOGRAPHS ON RADIOCHEMISTRY AND RADIOCHEMICAL TECHNIQUES

Available fromthe National Technical Information Service, U.S.Department ofCommerca. pringfield, 22161 S Virginia ELEMENTS

Recent Radiochemlcal Seoaratlon Procedures for As, At, Be, Mg, Ni, hu, and Se, NAS-NS3059 [19741 , Alumlnum and G.sllium, NAS-NS-3032 [1961]

$5.00

, ,

$4.50 Americium $4.50

and Curium,

NAS-NS-3006

[ 1960]

Antimonv, NAS-NS-3033 [ 1961] , $4.60 Arsenic, NAS-NS-3002 (Rev. ) [1965] , $3.60 Astatlne, NAS-NS-3012 [ 1960] , $4.00 B.srlum. Calclum. and Strontium. NAS-NS-301O [19601 ,$5.50 BarVllium, NAS-NS-3013 [19601 , $4.50 Blamuth. NAS-NS-3061 [19771 . $4.75 Cadmium, NAS-NS-3001 [ 1960] , $4.50 Carbon, Nitrogen, and OxV#en, NAS-NS-3019 [ 1960] , $3.60 Cesium, NAS-NS-3035 [ 1961] , $4.50 Chromium. NAS-NS-3007 (Rev.) [1963]. $4.60 Cobalt. NAS-NS-304i [ 1961] S5.00 COPPe;, NA-S-NS-3027[ 1961] ,-$4.50 Fluorine, Chlorlne, Bromine, and lodine, NAS-NS.30~ [ 1960] , $4.00 Francium, NAS-NS-3003 [1960] , $4.00 Germenium, NAS-NS-3043 [ 1961] , $4.50 Gold. NAS-NS-3036 I 19611. .S4.00 Indlum, NAS~NS.3014 [ 19601_, $4.50 Iodine, NAS-NS-3062 [1 977] , $4.75 Iridium, NAS-NS-3046 [1961] , $4.00 Iron, NAS-NS-3017 [1960] , $6.00 Leed, NAS-NS-3040 [ 1961] , $6.75 Megnedum, NAS-NS.3024 [ 1961] .$4.00 Manganesa, NAS-NS-3018 (Rav. ) [ 19711, S4.50 Mercury, NAS-NS-3026 (Rev.) [1970] , $7.76 Molybdenum, NAS-NS-3009 [ 19601, $4.00 Neptunium, NAS-NS-3060 [1974] , $8.00 Nickel, N:j::om NAS-NS-3051 [1961] , $6,00 end Tantelum. NAS-NS-3039 [ 1961] ,

Selenlum, NAS-NS-3030 (Rev. ) [ 19651, $4.50 Silicon, NAS-NS-3049 (Rev.) [ 1968], $5.00 Silver, NAS-NS-3047 [19611 , $4,50 Sodium, NAS-NS-3055 [1962], $4.00 Sulfur, NAS-NS-3054 [ 1961] , $6.00 Technetium, NAS-NS-3021 [ 1960], $4.50 Tellurlum, NAS-NS-303E [ 19601,$4,00 Thorium, NAS-NS-3004 [19601 , $4.50 Tin, NAS-NS-3023 [1960] , $4.50 Titenium, NAS-NS-3034 (Rev. ) [ 1971] .$5.00 Tranwurium Elements, NAS-NS-3031 [1960] ,

$4.00
Tungsten, NAS-NS-3042 [1 961] , $4.00 Urenlum, NAS-NS-3050 [19611 , $10.60 Venadlum, NAS-NS-3022 [ 1960] , $5.00 Zinc, NAS-NS-3015 [1960] ,$4.50 Zi:40;&m and Hafnium, NAS.NS.3011 [ 19601,

TECHNIQUES
Absolute Meamrement of Alphe Emlaslon und Spontanaoua Fission, NAS-NS-31 12 [1968] .$4.50 Activatlo& Anal Vsi~ with Chargad Particles, NAS-NS-3110 [19661 , $4.00 Applications of Computers to Nuclear and Radiochemistrv, NAS-NS-3107 [19621 ,$9.75 Application of Distillation Technlquea to Radiochemical Separations, NAS-NS-31 06 [1962] ,$4.00 CarIon-Exchange Techniques in Radiochemisnry, NAS-NS-3113 [1971] , $7.5o Chemicel Yield Determination in Radlochemlstrv, NAS-NS-3111 [1967] , $5.50 Datectlon and Measurement of Nuclear Radiation, NAS-NS-3105 [1961] ,$6.00 Liquid-Liquid Extraction with HighMolecular-Weight Amines, NAS-NS-3101 [1960 ],$5.00 Low-Level Radiochemlcal Separations, NAS-NS-3103 [19611 , $4.00 Neutron Activation Techniques for the Measurement of Trace Metals in Environmental Samples, NAS-NS-3114 [1974] , $5.00 Paper Chromatographic and Elactromlgratlon Techniques in Radiochemistrv, NAS-NS3106 [1962], $4,50 uf Counting Data, NAS-NS-3109 Processing [1965] ,$6.75 Rapid Radlochemlcal Separations, NAS-NS3104 [1961], $6.00 Saparetions bv Solvent Extraction with Trl-n-ocWlphosphlne Oxide, NAS-NS-31 02 [1961 ], $4.50 Users Guides for Radloactivltv Standards, NAS-NS-3115 [1974] , $5.00

Osmium, NAS-NS-3046 [1961] , $3.50 Pelladium, NAS-NS-3052 [ 1961 ] , $5.50 Phosphorus, NAS-NS-3056 [1962] , $4.00 Pletinum, NAS-NS-3C144 [ 1961 I , $4.00 Plutonium, NAS-NS.305B [ 1965] , $7.50 Polonium, NAS-NS-3037 [ 1961] , $4.60 Pomaslum, NAS-NS-304B [ 19611, $4.00 Protactinium, NAS. NS-3016 [1959] , $6.00 Radium, NAS.NS.3C)57 [lg64j ,$7,75 Rare Earths-Scandium, Yttrium, and Actinium, NAS-NS-3020 [1961] , $9.25 Rare Gases, NAS-NS-3025 [ 19601, $4.50 Rherrlum, NAS-NS-3028 [ 1961] , $4.00 Rhodium, NAS-NS-300B (Rev. ) [ 1966] ,$5.00 Rubidium, NAS-NS-3053 [ 1962] ,$5.00 Ruthenium, NAS-NS-3029 [ 1961] , $5.00

Current

as of

March

1978

AEC Cete@ry
UC4

NAS-NS-3035

The Radiochemistry

of Cesium

H. L. FINSTON
Brookhawn Upton, New

and M. T. KINSLEY

Naticnzul Laboratory York

February 1961

Reprinted the by Technicel Infornurtion Center U,S.Departnwnt ofEnergy

Subcommittee on Radiochemistry National Academy of Sciences National Research Council

.. . .
,-

,..

AVAIL AS t4AS-iJS-3035 Fall $9+75 FROM NATXGh!AL TECHNICAL INFORMATION U+S+ DEPARTMENT OF CC)KHERCE SPRINGFIELD LJI% 22161

SVC

Prirrta+l intheUnittiStaWd Arimfice

USDOETahriical lnforrnetion Cent&, Oak Ridee,Tenfi 1961; Iatastprinting March 1976

FOREWORD

The Subcommittee on Radlochemlstry 1s one of a number of subcommittees working under the Committee on Nuclear Science within the National Academy of Sciences - National Research council . Its members represent government, indu6trlal, and university laboratories In the areas of nuclear chemistry and analytical chemistry,

The Subcommittee has concerned Itself with those areas of nuclear science which involve the chemist, such as the collection and distribution of radlochemlcal procedures, the establishment of specifications for radlochemlcally pure reagents, availability of cyclotron time for service Irradlatlons, the place of radlochemistry In the undergraduate college programJ etc.

This series of monographs has grown out of the need for up-to-date compilations of ra.biochemical information end procedures. The Subcommittee has endeavored to present a series which will be of maximm use to the working scientist and which contatis the latest available information. Each monograph collects h one volume the pertinent information required for radiochemlcal work with an individual element or a group of closely related elements.

An expert h the radiochemistry of the particular element has written the monograph, following a standard format developed by the Subcommittee. The Atoml.c Energy Commission has sponsored the printing of the series,

The Subcommittee is confident these publications will be usefti not only to the radiochemlst but also to the research worker in other fields such as physics, biochemistry or medicine who wishes to use radiochemlcal techniques to solve a specific problem.

W. Wayne Meinke, Chairman Subcommittee on Radiochemistry iii

INTRODUCTION

The series of monogra@m3 k-ill cover all elements for wliich plana include revlslon ra.iloctiemtcai proceatires zrz psrtinetit. of the monograph perlodlcaiiy aa new- technlquea an.i prGee[iurea W-arrzmr The rezfler la tkierefors encouraged to caii to the . a~ten~ian ,of t:ne author any pu-liisrle.i or uripu-iilahe.i material on t:ne rzmiiocr,erl~stryof cesliim-w-rllcr! mlgnt be inciudecd In a revlaed v?raion Gf th~e monograpli.

iv

CONTENTS

I.

General Reviews of the Inorganic Chemistry of Cesium Table of Isotopes of Cesium

and Analytical

II. III .

3 Chemistry of 6

Review of those Features of Cesium Interest to Radiochemists General Properties Cesium Metal Halides Oxides Hydroxide Cesium Permanganate Chromate Permolybdate Sulfates Polysulfides Nitrogen Compounds Salts of Oxides of Phosphorous Carbonate Analytical Methods

6 6 8

11 12 13 14 14 14 17 18 19 20 21 Compounds of 27

IV.

Dissolution Ces ium Counting

of Samples

Containing

v. VI. VII.

Techniques

Eor Use with

Isotopes

of Cesium

29 32 35

Applications Collection for Cesium

of Radioisotopes of Detailed

of Cesium Procedures

Radiochemical

TABLES

I.

Atomic

and Physical

Pro~erties

of Cesium

II. III. IV.

Properties Properties

of Cesium of Ceeium Metlmda Methoda

Halides Pemanganate

9 1-4

Precipitation Carrier-Free Ion Exchange

22 24 Methoda ~=J 26 30

v.
VI. VII. VIII.

and Chranatographic Methods Yields

Spectrochemical Fission Product

FIGURE I. Decay Scheme of Cealum-137 31

VI

The Radioc,hemistry
1% L. FINSTON
IWookhaven

of Cesium

and M. T. KINSLEY
National Laboratory York

Upton, New

I.

General Reviews Qf Cesium

of the Inorganic

and Analytical. Chemistry

Furman,

N.H.,

cd., Scotts 1, 893-8,

Standard

Methods Co.,

of Chemical Inc.,Mew

Analysis, 1939.

5th Ed., Vol.

D. Van Nostrand

York,

Hillebrand, Applied

W.F.,

Lundell, Analysis,

G.E.F.,

Bright,

H.A.,

Hcxffman, J.I., & Sons,

Inorganic

2nd Ed.,

646-70,

John Wiley

Inc., New York,

1953.

Jacobson, 618-60,

C.A., Encyclopedia Publishing

of Chemical

Reactions, 1948.

Vol.

11,

Reinhold

Co., New York,

Latimer,

W.M.

and Hildebrand, Ed., 36-56,

J.H.,

Reference

Book

of Inorganic

Chemistry,

Revised

Macmillan

,CO., New I!ork, 1940.

Noyes,

A.A.

and Bray,

W.C.,

Qualitative

Analysis

fc)r the Rare 1927.

Elements,

245-67,

469-79,

Macmillan

Co., New York,

Sneed, Vol.

M.C.

and Brasted,

R.C.,

Comprehensive

Inorganic Co.,

Chemistry, Inc.,

6, The Alkali 1957.

Metals,

3-182,

D. Van Nostrand

New York,

Thorne,

P.C.L.

and Roberts, Publishing

E.R.j

Fritz

Ephraim

Inorganic 1943.

Chemistry,

4th Ed., Nordeman

Co., Inc., New York,

West,

T.S.,

65, 467-70, Chem. Age

473,

1951.

(68,84) 11. TABLE OF ISOTOPES OF CESIUM

Isotope ~s123 ~s125

1/2 6m 45 m

TYP e of Decay

Energy of Decay Particles Mev (relative intensities)

Formation

9+
E. C. 82% E. C. 18%

1127 @+ 2.05 Y 0.112 ~+ 3.8 0.385 Y ~+ 0.68, 1.06 y 0.125(10),0.286(?) 15 0.406 (80),0.440(Weak) Q+ 1.5 (3),2. 5(30), 3.()(7CI) 0.445,0.980 ; y 0.04(460)*,0.092(11.4)*, 0.174(0.35)*,0.283(1.36) *, 0.315 (d. 2)*,0.371(13.2) *, o,411(w10 )*,O.545(O.52)*, 0.585(w0.22)* intensities *relative Ce k ~+ 1.97(28) ~- 0.442(1)

(z,6n) 126

~s126

1.6

6+

Daughter

Ba

cs127

6.25 h

P+
E. C. ~

127 Daughter Ba 1127(u,4n)

cs128

3.8

P--75%
E. C. 25% E. C. no E

Daughter

Ba

128

cs129

31

Daughter Ba I127(a,2n)

129

~s130

30

P+

1127

46% E. C. 52% 9- 1.6%

(a,n)

11. TABLE

OF ISOTOPES

OF CESIUM

(Continued)

Isotope ~s131

1/2 9.9 d

TYP e of Decay E. C. no ~+

Energy of Decay Particles Mev (relative intensities)

Formation Daughter Ba 13a130(n,ye) 1127(a,Y) ~s133 131

6.2

E. C. +98%

0.670(100),1.08(0.6), 1.20(0.6),1.30(1)

(n,2n) Cs133(25-Mev

p,pn)

Stable 3.1 h

100% abundance CS133 IT 99% p- % 1% @- -0.55 0.0105(98%),0.127(98%) Y 0.137(0.8%) , (n,Y) cs133(d,p) ~s133

/=-

~s134

2.2

~-

9?

0.083(32%),0.31(5%), 0.665(50%),0.683(13%), 0.473(1.8),0.563(9), 0.569(13),0.605(100), 0.795(91),0.801(18), 1.038(0.9),1.168(3.0), 1.367(4.6) 0.21

(njY) cs133(d,p) Ba136(d,a)

~s135

2.0X106 y

9-

6PY

Daughter U(n,f) La139

Xe

135

~s136

12.9

D-

0.341(92.6%) 0.657(7.4%) 0.0672,0.153,0.162, 0.265,0.335,0.882, 1.04,1.245,1.41, 2.35,2.49

(n,a) U(n,f)

30

@-

9Y

0.514(92.4%) 1.18(7.6%) 0.662 (with Ba 137m)

Daughter U(n, f)

Xe

137

32

3-

3- 3.40 r 0.139(2.0%),0.193(0.8%), 0.229(1.6%),0.411(3%), 0.463(23%),0.550(8%), 0.87(4%),1.01(25%), 1.43(73%),2.21(18%), 2.63(9%),3.34(0.5%)

P4.3

Descendant 1138 Daughter xe138 Ba138(n,p) U(n,f)

9.5

@-

139 Daughter Xe Descendant 1139 U(n,f) Daughter U(n,f) Daughter U(n,f) Daughter Daughter Xe Xe 143 144 Xe 140

Cs

140

66

P-

~s141 ~s142 Cs 143

short W1 short short m

DPDP-

Xe

141

c~ 144

III.

Fe atures E~View of t~e to Radiochemists

of Cesium

Chaistrv

of Interest

GENERAL Cesium the members and those with is a member

PROPERTIES series M4-K-R&Cs

of the homologous similarity

of which

show greater

in their properties of any other The element with group is the

of their

compounds exception in nature

than the members of the halogens. almost always amounts.

the possible distributed alkalis

widely other

associated

and usually occurs

in small

The highest

concen-

tration contains

of cesium little

in pollucite

(34% CS20) which is obtained contain

generally

or no rubidium.

Cesium

from the

carnallites percentages in the large

of the Stassfurt of cesiun scale

region

which but

only small

and rubidium,

these

are concentrated

extraction

of potassium. METAL in the pure state but of small is amounts

CESIUM The metal frequently is silvery yellow

white

a golden

due to the presence

of oxide or nitride. Cesium is the most active and the most l.Gu;~- Im electro-p P sitive of all the metals, and on exposure to air it tarnishes or bursts metal. detected -108C Metallic quickly and melts due to the formation atomic of Impurities volume cannot of any be with

into flame.

It has the largest cesium

The reaction between at temperatures

and moisture

below

-116c;

this may be caupared and -98C

for rubidiun, cesium

-105C

for potassium, interest

for sodium. of

is of greatest

for the manufacture advantage

photoelectric its range

cells;

it possesses

the greatest closely

that

of sensitivities

corresponds 6

to that of the

human

eye.

The properties

of the metal

are summarized

in Table

I.

The metal was the electrolysis of magnesiun

first prepared

by Setterberg

in 1881, by The action

of a mixture

of CSCN and Ba(CN)2.

or rare earth metals suitable

in the form of Miscpmetal of metal from

is particularly

for the preparation

Table Atomic Atcinic weight Atomic Melting Boiling Density, number pOint,C pointJOC 20C [ Neutrons [ Protons(+) in VariOuS quantum and Physical

I of Cesium(Cs) 132.91 55 28.4 690 1.90 78 55

Properties

ucleus Electrons

levels:

1st 2nd 3rd 4tl-1 5th 6th

2 8 18 18 8 1 3.87

Ionizing

potentials

of gaseous

atoms,

volts

Potential required to remove frcan solid metal

electrons

Potential between metal and normal solution of ion; M = Maq+ eHeat Ionic of hydration radius of gaseous

aqueous 3.02 63 1.69

ions, kcal 8

in crystals,

an x 10 x

ceaium heating

oxide.

The metal

has also been or by heating

prepared CSC1 with

frcm CS2C03 by calciumi chips of cesiiun have electrodes; ceslti

with magnesium;

in a strean.of been prepared have

dry hydrogen.
In ether

colloidal

solutions

by arcing formed

two noble metal

aerosols is bluish

also been closely

in gases.

The colloidal

green,

resmbling HALIDES

the color of Ehe vapor.

Cesium zation alum.

chloride

can be obtained contains

by prolonged

recrystallisoluble cesium with HC1 to

of carnallite , which A preferred

the slightly

preparation follmed

consists

of precipitation with gaseous

silicomolybdic volatilize to separate made

acid,

by treatment

molybdenum the other

and fractional chlorides.

crystallization

from aloohol are

The branides with

and iodides

from the hydroxide mixtures

by treatment

free halogen;

this

yields

of Iodate-iodide

and brmnate-branide, and iodate

respectively. are

The mixtures reduced,

are evaporated

and the branate carbon

e.g., by heating halides

with

or in a stream cubic with

of H2S.

Cesifi of CSF which follms (A):

are body

centered the sides

the exception are as

is face centered;

of the cubes

CSF Cscl CsBr CSI In contrast halides

6.01 4.12 4.29 4.56

(face centered)

to the other

alkali

halides

the volubility

of cesium of

decreases

fran chloride

to iodide; II.

the properties

the halides

are summarized

in Table

Table

II

Properties Melting Boiling Heat point, point, C C

CSF 683 250

Cscl 626 1303 39.750

CsBr 627 1300 36.070

CSI 621 1280 44.820

of vaporization,

kcal

kcal/rnole Heat of dissociation, (MX M~a~ + X~a~) InterIonic distances Measured, A Calculated, Critical A (talc.),c (x 10%)

98.9

99.0

100

3.06 3.07 2421

3.14 3.18 2433

3.41 3.43 2407

temperature g/100 Oc

Volubility,

g H20 366.5 (10) 161.4 123 {25) 44

100C

270.5

160 (61) 97.65 83.90

Heat

of fonnation,kcal/mole

106.32

Polyhalides Cesium, polyiodides cesium orating because of its large stable atcmic volume, easily forms The evapsalts a

which

are very CSI 3

and fairly

insoluble.

polyiodides, a solution

and CS14,

can be formed by simply The analogous There branine

of iodine

in CSI.

are also known, considerable CsBrC12, solutions

but not the chlorides. of mixed These polyhalides;

are, however, CsIBr2,

number

e.g., readily in color

CS1C12

CsClBr2. of their

all crystallize and range

frcm aqueous frcm the black yellow

cmponents through

of the polyiodides

bichromate-oran9e stability 9

to the pale

of the bran-chloride.

Their

is considerable,

CS13

reaching Another

a decomposition halide, CSIC14,

pressure

of 1 atmosphere

only at 250c. as

is also known

and may be considered with iodine

the addition It can be

compound

of the chloride ways

trichloride. solutions chloride, of

formed

in various

from the aqueous and iodine

the ccnnponents, e.g., from the iodate acid. It exists

from the chloride

and chlorine,

or from iodate needles

and hydrochloric upon exposure to

as fine yellow trichloride.

which,

air, give Ccmplex

off iodine

Halides Cesium also forms canplex halides which are frequently in the detecof such

difficultly

soluble

cmnpounds

and which

may be used metal.

tion or estimation

of the accompanying 5;

Examples

ccsnpounds are: Cs3SbCl yellow Cs2NaCo(N02)6 transparent

4CsCl4SbC13.FeC13; of detecting crystals

red CS Bi I . 229 0.01 mg of Co;

capable

Cs31nC16,

octahedral

capable

of detecting

0.02 g of In; Cs2PbCu(N02)6, corresponding a bright nickel compound

employed used

to detect

Pb or cu and a ) 2 30 2

to detect

Ni; Cs9Bi5Na6(N0 0.02 mg of NaNO or other

yellow

ccrnpound capable

of detecting

in the presence metals; Cs2TeC16,

of TIJ Zn, Cd, alkaline lemon

Yellowj

earths,

alkali

sensitive white

test for Te, applicable Ca2ptCl ~, yellow;

CS2M62Fe2(cN) ~2

in the presence CS2CUHgC16; Perchlorate

of Se; Cs2SnC14, CsAg2Au2C112;

crystals;

CSAUC14;

CS4ZnAU2C112;

The general extent on the large ion.

propertiesof volume

perchlorates

depend

to a large of the atmnic

and symmetrical of metals

structure large

perchlorate volumes

Perchlorates

with

(K, Rb, and Cs) are not greatly

hydrated;

consequently,

10

cesium

perchlorate,

CSC1O ~, is sanewhat
The

insoluble

(1.6 g in reduced

100 g of water

at 20C).

volubility

is considerably

in ethanol

solution

at OC. is prepared by evaporation of an app~oprie.g. ,

The perchlorate ate salt with

pert-nloric acid, by heating 4CSC103 4CEC1 of weakly + 3CSC1O 4 acidic

the chlorate,

and by anodic latter ate; 1-

oxidation yields

chloride

solution.

The

technique

first the chlorate emf, and high

and then the perchlordensity favor

temperature,

high

current

the formation Periodate

of perchlorate.

The periodates the perchlorates; and oxygen. with chlorine

are in general

significantly

different into iodates

frcm

on heating

they are decomposed are produced

The periodates or by anodic

by oxidation acidic

of iodates or alkaline are

oxidatia

in either a lW

solution, desirable. CS104 Cesium

but a lW All

temperature,and

current

density

the periodates to the extent

are slightly

soluble

in water: at 15G

iS SolUble forms

of 2.15 g in 100

3 of water pe~iodic 1

the only knwn

salt of fluorinated are knmn, nor

acid;

no other iodates

fluorinated and brcxnates.

halogenates

are chlorinated

OXIDES The and CSO following oxides of cesium are known: cs20cs202J cs203J

.2 r cs204 Alkali metal oxides show an interesting weight increases. of metal gradation The ratio in of oxygen

stable

types

as the atanic

to metal

increases

as the radius

Incpeases;

thus the

11

stable calcium

oxide

of cesium

is the superoxide, and should

CSO 2

It has

the

carbide

structure CS20,

not be called

tetraoxide.

The oxide, decompose Cesium with

vaporizes

markedly

at 250c and tends to temperatures. decomposes Ammonia

into metal

and the peroxide in excess o~gen to yield

at high yields Cs203

upon burning

CS204 which and oxygen.

difficulty

upon heating

solutions with

of the metal

are deep blue

in color

and w-hen reacted settles is conand

oxygen,

a colorless

or pale pink bulky

precipitate

out while tinued,

the solution

is decolonized. becomes

If the reaction brown color

the precipitate

a chocolate CS203

corresponds

to the composition melts yellow agent

at the maximum

coloration. further is a by

It is crystalline, oxidation strong water yields

upon heating needles

and turns black; The peroxide

of CS204. skate

oxidizing with

in the fused

and is decomposed

the formation

of H.Oa and On.

L4 4

HYDROXIDE Cesium thesis hydroxide, hydroxide CsOii, can be easily and cesium prepared by meta-

of barium

sulfate;

alternatively

the cheaper

slaked CS2C03

lime may be used, L + Ca(0H)2 v 2CS(OH) reactions

+ CaC03 consequently, in this manner. method it is Elec-

Both

of the above

are reversible,

not possible trolysis

to prepare

the pure hydroxide is the principal The anode

of cesium

chloride

for preparacompart-

tion of pure hydroxide ments method method are isolated employs

solution.

and cathode ways;

from each other cement

in various

the diaphragm the bell 1 arm

a porous

or asbestos

diaphragm,

can be described

as electrolysis 12

tube with in a ,,uc,

constituting mixing plating

the anode

and the other

the cathode consists cathode

so that no essentially
on one

occurs, cesium

and the mercury fran brine

method

of

into a mercury

side of

a U-shaped side,

apparatus

and this then beccnnes an anode is stripped. is a highly readily alkali deliqueacent,

on the other

from which

cesium

Cesi.um hydroxide solid (density heat. = 4.018) The fused

crystalline the liberation due to the

soluble attacks

in H20 with manymetals

of much

formation canbines oxidation oxides

of small quantities with oxygen

of the free alkali peroxide

oxide which causing have acidic

of the air to yield Metals

of the metal.

like platinum to attack. CSOH, When

which

are particularly When ozone

susceptible over

is passed

solid

the white

solid

turns

orange

and fixes

2.2% of the oxygen. oxygen is given

the resulting

canpound not

is wetted, as ozone, the orange remains. indicating

the fixed and 0 22

off aa Inactive solution. color

oxygen

is given

off upon

On standing, of the peroxide with H20

color disappears The aged substance

and the yellcw yields H202

on treatment

conversion

to peroxide CESIUM

hydrates.

PERMANGANATE of rubidium and cesium are prepared solution of

The permanganate by adding potassium

salts

the corresponding permanganate

nitrates

to a saturated

at 60c. salts.

On cooling,

they crystallize CsMnO 4 is the

out as the anhydrous least soluble with

Cesium

pennanganate,

of all the alkali increasing atmic

permanganates, volwe

the volubility to the behavior are

decreases

analogous

of the perchlorates.

The properties

of cesium

permanganate

13

summarized

in the Table

III. Table III 3.55 temperature 320c 0.097 0.23 1.25 ~~ (lc) (19c) (60c)

Density Decanposition Volubility,

g per 100 g solution

Saturated

cHRa4?iTE Cesium alkali metal chranate, chranates Cs2Cr04, is the least those soluble of the and of

and restiles crystallized.

of potassium salts

rubidium these more

in being

easily

The normal

elements rapidly

differ

fran that of sodium salts and yield

in that they dissolve the anhydrous salt.

than the acid

PERMOLYBDATE Cesium the fact that with metal a solution quite permolybdate, Cs20 4M004, is distinguished of all the salts by addition by formed to are

it is the richest

in oxygen

per-acids.

It can be prepared salt. All

of H202

of the normal

the alkali with

permolybdates

soluble

but can be precipitated SULFATES

alcohol.

Cesium of NH ++ 4K

sulfate,

CS2S04,

forms an anhydrous those of Na +

salt like those The soluIncreasing

+ and l?b and unlike (per 100 g H20) as follows: 2s04 7.35 g 24.1

+ and Li . with

bilities atomic

in this series

increases

weight

Temperature .

94 36.4 el.a

(NH4)2S04 71.0 97.5

cs2s04 167 220

0
100

14

Cesium

Alum Alum in general alUmS form a very have characteristic group of domle

salts. where

The CeSIUm M may be many

the formula, metals

CS[M(S04 )2]0 12H20, Cr, Fe, Co, ~, sulfate in

tervalent

such as Al,

Ir, Mn, !?, but not Bi, Tl, or rare the alum may be replaced in the regular Upon addition form,

earths. All

Also, alunw

by selenate. which

crystallize size.

octahetia,

may grow

to large

of various

substances

to the solution

(urea, borax) that

the growth cubical formed.

of the octahedral or other

faces may be so repressed system, slums

faces,

faces of the regular of the series

may be decreases used to solu-

The volubility to cesium

of alkali

fran sodium isolate bilities

alum

so that

the latter

has been metals.

cesium

frcun the mixtures

of the alkali

per 100 g of ~0

of sane anhydrous

slums

are as follows:

Temperature KA1(S04)2 NH4A1(S04)2

0 2.87 g 2.53 0.71 0.21

30 7.74 8.34 2.12 0.60

60 19.85 17.40 6=89 1.92

Melting (92.5) (95) (109) (122)

Point 54.45 52.20 58.5 62.0

RbAl(so4)2
CSA1(S04)2

Tne melting be noted Cs.

point

is the transition

point

of the alum. in the direction

It may K to

that this temperature

increases

An increase to favor

in atanic

volume

of the anionic canplex.

metal

seems to

the stability and,thus

of the anionic the vapor

The tendency of

lose water,

also

pressure

of the water The

crystallization,

rises with

decreasing

stability.

follming

15

table vapor

gives

the temperature of 300 mm:

at which

some ceaium

almns have a

pressure

Anionic Atomic Dissoc.

metal vo\ume(xlOB cm)

Al 10.2

Ti 9.3

v
8.8

Cr 7.7

Fe 7.1

Temperature (C) for 300 nnn

96.52

92

85

84

76.5

Schonites The cesium CS2M(S04)2* bivalent 6 H20, schonites in which correspond to the formula,

the M may be any one of various They soluble and of the similar canis

elements

such as Zn, Ni, Co, Fe, Cu, Mn, and V. monoclinic variety crystals and are moderately

form Isanorphous in water. they have, effect atans. pounds always

A great

of sctionites can be prepared studied in investigation lattice by other

consequently, atmns

been

of replacing It was

in a crystal in formation

found that elements,

of such analogous of contraction stable

fran their similar~

the percentage the more

but

it is greater the percentage canponents

the compound.

For cesium

schonites

contraction

in the formation

from the individual Double

is as follws: 6 H20 m 43.8 n 45.9 cd 43.4

sulfates Mg NI

of the type CS2M(S04)2 Co 45.4 Fe 44.8 Cu 45.4

% Contraction

46.1

46.0

Perr3ulfate Cesium pound; series persulfate, CS2S208, is a s~ringly soluble com-

the volubility K-ti-Cs-Tl.

of the persulfates

diminishing acid,

in the may be

The compound,

perdisulfuric

16

prepared

by electrolysis

of an acid anmmnium

sulfate

solution;

the reaction

is a8 follows: H2S208 + 20H-. is

2HSO; + %02 + H20 + In the presence obtained, of $ a higher

yield. of the psrsulfate

and in the presence

of Cs the cesium

persulfate.is

precipitated. Pyrosulfates These as a complex compounds compound have formed the formula M2S207 and may be regarded of water by free

by elimination

of one nmle

from two moles heating

of sulfuric

acid.

The salts may be formed the neutral sulfate with

the bisulfate, tube,

by heating

S03 in a closed
sulfate sulfates calcining,

or by recrystallizing sulfuric

the sulfate

or bipyro-

from warm are best

concentrated known;

acid. easily,

The alkali give

they dissolve

up S03 on

melt more

easily

than the sulfates

(below red heat), potassium, and.

and solidify rubidium earths,

in crystals

from the melt. those

Cesium, of sodium

pyrosulfates

are unlike

and the alkaline of the acid oxide

in that they take up SIX more molecules S03 and form crystalline compounds

in liquid M20

of the formula

eso3. POLYSULFIDES sulfides of metals giving having large atomic which volumes combine

with with

more

sulfur,

pelysulfides,

may be compared the alkali metals,

the polyhalides. cesium,

As In

the Wlyhalides, stable as high

especially

form the most which range

compmnds. as M2S5

Compounds are known. but

of the alkali

metals

The solid polysulfides

are well

crystallized

substances,

17

all except attacked course, between composed

Cs S 25

are very hydroscopic of the air when with

and are somewhat moist.

readily

by the oxygen decomposed sulfur

They are, of of equilibria are de-

by water

the establishment me persulfides of sulfur.

and lower

sulfides.

by acids with

the liberation NITROGEN

COMPOUNDS

Azides The best method makes gens use of nitrous CSNH2 + ON2 ~ of preparing the salts of hydrazoic acid

oxide

as the source 3.

of the combined

nitro-

H20 + cm

It is interesting

to note, azides by reWith K, of

although

it is not of practical synthesized

importance,

that alkali and nitrogen discharge.

may be directly action under

from the metal of the electric accompanied The azide

the influence

Cs, and Rb, azides nitrides alkaline well

are formed

by small quantities

as secondary earths,

products.

salts of the alkalis, metals are all The

lead and the univalent the halogen

heavy

known

and resemble

salts

in many

respects.

alkali

azides

do not explode

even on percussion as they explode of alkali

and may almost only at high

be melted

without

decomposition,

temperatures. arranged preparing azide

The decomposition

azides may be so a method for in the

that it takes place pure nitrogen at about

gradually

and gives This

or pure metal. 350c.

is observed

of cesium

Nitrites The property nitrites is applied nitrites of nitrates of the alkalis of decomposing 3 _+2CsN02 melt + Q 2. on heating to to

to their preparation:2CsN0 are strong electrolytes,

The alkali

18

yellow

liquids

which

decompose acid

at higher

temperatures,

and

hydrolyse nitrites

to nitrous

on boiling

with water.

T-he alkali

form only very

small

crystals

and are hydroscopic. varies considerably. compounds:

The stabj..Lityof complex To the weak Cs[Ag(N02)2]j complexes belong

nitrites

the easily

decomposed

cs2[ca(N02)4],

and Cs2Na[Bi(N02)6] of sodium

which serves

for the quantitative Nitrates Nitrates

determination

or bismuth.

are almost

exclusively

obtained

by the action
A1l

of

the free acid on metals, dissolve alkali easily in water.

oxides,

or carbonates.

known nitrates and the -1-

The volubility order

of ammonium Na +

nitratesin nitrates

decreasing

is NH+ 4 melt

IK+CS. on dry

The alkali heating.

are anhydrous, points

and decompose fusible

The melting are:

of some nitrates,

without

decomposition,

H4N03 Melting point 170

LiN03 2640

NaNO

KNo

IL!

sNO

Ba(N03)2 592

314

339

414 point

If several pressed.

of these

nitrates

are mixed

the melting

is de-

SALTS Hypophosphites (H2PO~)

OF OXIDES

OF PHOSPHOROUS

All the salts of hypophosphorous soluble in watex in contrast

acid

are monobasic,

easily

to the phosphates, and alkaline

and show reducing earth salts are

properties anhydrous

in solution.

The alkali water.

or contain . Phosphates (P03) Phosphates

little

of the alkalis

are soluble

in water,

all others

being

very

sparingly

soluble;

they

are not amorphous

like the mostly with

phosphates, a definite

but crystalline water content. (P206=) salts

like the hypophosphites,

Hypophosphates

The alkali phates

are soluble soluble.

in water;

all other salts

hypophosare

are difficultly in water. . (PO;)

The normal

alkali

hydrolyses Phosphates Only

the phosphates earths

of the alkalis

and the primary

salts of of

of the alkaline the normal the alkali, very

are soluble

in water. with

The volubility

alkali

phosphate

increases

the atomic weight

that of the phosphates On hydrolysis

of K+, Rb+, and Cs+ being they are almost and alkali cesium completely hydroxide. phosphate

considerable.

decomposed The water

into the secondary of crystallization

phosphate

in the tertiary

in the secondary = Pyrophosphates (P207=) The pyrophosphates neutralization 2H2p207 alkali

is 5 moles;

salt it is 1 mole.

are obtained

only in two stages ealts M4P207

of and

- as quaternary salts

and secondary

The alkali

are soluble

in water;

the quaternary

salts

are slightly

hydrolyses. CARBONATE

Carbonates of the metallic

may be regarded oxide and carbon

as cwplex dioxide metals

anionic

compounds

of the type M[O(C02)], are more stable the car-

and the carbonates greater bonates the volume there

of c-parable of the cation.

In the series

of alkali

is an exception

to the above

stability,

for the

20

dissociation increases show

of potassium

carbonate

is least,

and it then carbonates

to cesium

carbonate. dissociation a2c03 41

At 1200c pressures: W03 60

the alkali

the following Li CO 23 ca 300 Carbonates

K2C03 27

cyo3 95 in solution, nun Hg and even fonnaand are solu-

are strongly carbonates hydroxides.

hydrolyzed are largely The normal soluble;

those of the alkali tion of the alkali that of thallium less soluble tions normal

deccunposed with alkali carbonates

are scmewhat

the acid

carbonates

and are therefore

precipitated

from saturated dioxide.

of the normal carbonates

salts by passing

in carbon

The

of potaaaium, the acid

rubidium,

and cealum

are deli-

quescent

in air, while

salts are unchanged.

ANALYTICAL The analytical mine ceaium iaotopea

METHODS to separate and/or deter-

rnethoda utilized are listed

in Tables

Iv, V, VI and VII.

21

Table

IV - PrecLpitatlon

Methods

Precipitant Alum

Sample Water, prepared samples organic

Technique Radiochemical

Comments Separates cs from bulk alkali elements and mixed F.P. 9$% Recovery Cs3Bi219

References 32,97

Bismuth

iodide

Fission product,alkali solutions Fission product,alkali solutions

Radiochemical, gravimetric Radiochemical, gravimetric

58,60

Chloroplatinate

Precipitates NH4

K,RbjCs

32,79,88 91,92,97 100 42,64,77

w w

Cobaltinitrite

Low cone.F.P. in HnO or aqueous solutions&containing alkali nitrite nitrite Alkali Alkali solutions solutions

Radiochemical, gravimetric, carrier-free Gravimetric Gravimetric down to 3 mg Cs Radiochemical, gravimetric (5-200 mg cone.range) Carrier-free

Cs:K:Na:Co ratio ppt 0.1:2.0:0,9:1.0

in

Silver bismuth Sodium-lanthanum

Specific

for Ru and Cs

36,37 21

Accuracy -&0.2%j Rb and K do not precipitate

Dipicrylamine

Fission product,aqueous solution

Radioactive Cs carries on both Cs and K dipicrylamine ppt.

30,50,80

Thallium (I) Dipicrylaminate

Fission

products

Carrier-free Cs can be extracted from precipitate. 90% recovery of active Cs.

101

Perchlorate

Fission

products

Radiochemical

Large amounts K,NH4 Na, and ~ interfere. Volubility product at lC is 1.5X1O-5. m coprecipitates. CS:NH :P:Mo ratio in ppt f.13tl.2:1.o:12. o 9376 recovery. Separates Cs from alkali metals. Cs2SnBr6 precipitate.

42,62,92

Permanganate

Aqueous solutions

Gravimetric

11

Phosphomolybdate

Low cone.F.P.

in H20

Radiochemical

42

Silicotungstate s Stannic branide Tetraphenylboron

Fission

products

Radiochemical

42,62,91

Alkali Fission

solutions products

Gravimetric Radiochemical

22 28,31

Macro amounts of Rb and K interfere.

Table V - Carrier-Free

Metho5s

Concentration Tracer Cs isotopes

Sample Fission products

Technique

Comments

References 101

Coprecipitake Active C% extracted with thallium into 2 N HC1. (1) dipicrylaminate Coprecipitate with NH4C10 4 High purity obtained. Cs tracer

Tracer Cs isotopes m
$=

Fission

products

63

Tracer Cs isotopes

Fission

products

<0.5% radioactive conCoprecipitate with ammonium lamination of tracer cobaltinitrite Cs isotopes. BaC12 precipitation. Solvent extraction using 0.2 M12 in nitrobenzene Tetraphenylboron e-xtraction Radiochemically pure c~131 obtained. Extraction coefficients 10-20 at 25C.

64

Tracer Cs13 -7

Irradiated

Ba

49,61

-10

to

10-3M Cs

l?urex type and T13P-25 type wastes

53

Tracer

to 10 mg Cs

Fission

products

See procedure

8.

23

Table VI - Ion Exchanqe and Cti~at09 raphic MethodE Resin Amberllte IFfA-400(@ Deacidite FFI Dwex-1 Dowex-1 Dowex-1 Sample F.I?.in acid F.P. in acid -pH 1 l?.p.in acid F.P. in 0.5% m4Cl Alkali metals in RDTA Mixed F.P. h H3P04 Eluant for C6 H20 None None None None None Cmmnents Sr,Cs eluted. F.P. held. Cs isotopes pass thrui Alkali metals pass thru. C. + Sr pass thru. Effluent order Cs-Na-Li. Cs, Te(IV) isotopes pass thru. Cs isotopes eluted. cs + few % M eluted. 5,57 99 65 24 Reference

Do-~ex-50 G Dowex-50 Dwex-5 O Duolite C-3

F.P. In HC1 and HN03 Alkali chlorides In H20 Low cone. F.P. in H20 High cone. alkali salt Solutio 2 Cs+10Na+5Rb Cs fraction separated frcm F.P. Activated alkali metals Separated K-I&cs fraction

0.50 N NH4C1 0.3 N HC1 6 N HC1 6 N HC1

99.7% Csrecovery. Cs + tiaceK + trace Na+ <2 ppm Rb eluted.

Duolite C-3

3 N HC1

Separates Cs isotopes frcm K and Rb Effluent order Na-K-Rb-Cs Estimates 5 to 1000 ~g of each cation. No interference frcm 1 mg Na,Li,Ba, Cs,Sr,llgu See Radiochemical Method 10 B 54

IR-1 Paper chrcxnatography

0.1 N HC1

Paper chrmnatography

Fission products

15,16

Table VII - Spectrochemical Spectral Lines .& 8!521 Determination Limit 8 ppm

Methods

Method Arc excitation

Sample Uranium base materials Silicates

Accuracy

Comments Carrier-distillation a203 Carr=er method.

Ref s 78

Arc excitation m m Hydrogen-Oxygen Flame Hydrogen-Oxygen Flame Image-Converter Flame Mass Spectrometry

8521

2 ppm

-5%

Methods for Na and K internal standards and for no internal standard are discussed. Spectrophotometer for radioactive designed samples.

Aqueous

8521

1 ppm

-1%

44

Glass,

Ores

8521

-1 ~g

Samples decomposed and dissolved in-O.02 N Hcl. 5-lo% Betteroprecision 8521 A line. with

93

Bi-U Alloys

4555,8521

O. 2-5%

90

Cs Isotopes

Isotopic Analysis

Cs isotopes obtained from fission product samples,

57

Iv.

Dissolution

of SmPle9

Containing

compounds

of Cesium

A prime subsequent

requisite

when with

dissolving carrier

radioactive

samples

for

determination isotope

is complete
Since

exchange

between in

the radioactive

and the carrier. there

cesium

exists

only one oxidation Another requisite

state,

is complete, remain

rapid

exchange. solu-

is that the isotope Cesium, adsorbs when

in homogeneous

tion until

analyzed.

present

in solution

in extremely

low concentrations, containers.

on the walls (16) have

of glass reported

and plastic that over has been 5W lost

Crouthamel, cesium-137 after

one

et al.

of carrier-free from solution mately

in 2 M HC1 or 2 M EN03

month,

and that the addition stabilized

of approxisolutions for

1 Ug cesium

carrier

per ml has

these

for a period cesium nuclear organic

of sti months.

Radiochemists types

generally

analyze irradiated sources,

isotopes

in the following cesium

of s=ples: natural water

fuel, activated materials,

salts,

and agricultural of irradiated using

materials. nuclear fuel elements pre-

The dissolution sents many It is very problems important

when

cesium-137

as, a burn-up

monitor.

that the section sample. parts

dissolved

is representative the neutron

of the entire flux varies

fuel element

In casei where

for different

of the sample, samples

the entire sample a

should be dissolved burn-up cesium map.

or sufficient must parent

run to determine prevent

Precautions

also be takento xenon.

loss of

and its volatile ~rosityof factors

The degree

of burn-up, of container Rider (75) for dia-

temperature, are important reported

the fuel,

and permeability problem.

in this contai~ent which indicate 27

two experiments

the necessity

solving

the container

in addition under

to the sample.

When

a small leached when

U02 piece was -out of Uo 2

irradiated

NaK,

75% of the cesium-137 measurements. Second,

relative

to gross

gamma

U308 was fission depth plete

irradiated products

in platinum driven

capsules,

cesium-137

and other

were

into the platinum

to sufficient effected com-

that only complete recovery. Fuel element

dissolution

in aqua reyia

samples 3

are generally

dissolved of these

in volatile acids, metal, or alloys

acids

such as HC1, HNO

HI?, or combinations of inactive cesium.

containing

a small amount alloys

Uranium

U02 , and U-MO

have been heated

dissolved

in concentrated (46,75) u-l%

8 N H.N03, gradually have been dissolved

in glass

beakers. HN03

in concentrated (46)

containing

a few crystals

of ammonium have been while other

bifluoride.

Other U alloys

(Al, gr, Mo, etc.) acid and

dissolved

heating metallic

in aqua regia containing 2% fluoboric ,--gradually. 1>) Zircalloy, stainless steel, clad fuel elements have been dissolved

in acids

in a similar Since their very

manner. all cesium is simple. salts dissolve Natural water in water sources and dilute generally acids, contain of

solution small

amounts

of cesium

isotopes

requiring methods.

concentration The preferred resin

the sample method column large

by either

of the following through

is to pass

the sample

a cation-exchange with

and then to elute concentrations

the cesium ions

6 M HC1. (41,42,98#1f with the ion-exchange Cesium (42) can be

of other

interfere

method,

then precipitation as cesium

methods

can be used.

precipitated

monium

phosphomolybdate

or copre-

28

cipitated

with

sodium

potassium

cobaltinitrite. human

(42,85,98) / urine, and blood, and, can be

Organic

materials, with

such as tissue,

can be decomposed follwi.ng extracted Cereals, 400-450C,

HN03

in the presence matter,

of carrier the cesium 7) .

destruction with water dried

of the organic or acid

(see procedure milk

(97,102,103) at

vegetables,

and&y

can be dry ashed hot HC1

and the cesium or hot HN03.

extracted (97) soils

with

(see procedure treated with

~), (102,103) M ammonium decomposed Cesium

are generally

acetate, with

the extr,act evaporated,

the organic

matter (102,103) (29)

HC1 or aqua regia, leached

and the cesium

extracted. IN HN03,

has also been N HF,

from soil samples (40)

with

3 N HC1-O.1 cesium values. . v. Countinq

(27)

or 9 M H2S04.

The naturally determining

occurring recovery

in soils must be accounted

for when

TechniW

es for Use with of measurement

Isoto PSS of Cesiiun of nuclides

The methods vary with such ation

of the radioactivity emitted

the properties as half-life,

of the radiations

by the nuclidee. of radi-

factors

type of radiation, The nuclear

and energy

must be considered.

characteristics

of the

isotopes

of cesiurn can be found in Section II.

in the literature

(68,84) and

are summarized

References details urement

for counting Surveys sources

techniques of general

should

be consulted

for

of the methods. of radioactive (83)

methods

for the meas-

are given

by -

and Seliger (52) scintillation 01son.(69) has been discussed

and by Steinberg. spectrometry Absolute

tie technique described

of gamma-ray (33) -d

has been

by Heath

calibration

of scintillation

crystals

29

by Bell. 81)

Pate and Yaffe

(70,71)

have described the 47T~- countrates. cesium-132

ing technique for determining absolute disintegration The isotopes of cesium from cesium-123 through have relatively short half-lives

and are not generally encountered.

Stable cesium-133

(u 0.016 + 31 barns) can be activated by thermal The preferred windowless

neutrons to produce cesium-134 m and cesium-134.

methods for the routine assay of cesium-134 are 2~counter and well-type scintillation counter. (51)

Pure cesiun-134

has been standardized by gamma-ray gamma photo-peak. (45)

spectrometry using BOO-kev

Fission product yields of cesium isotopes with half-lives longer than one hour are listed in Table VIII: (43)

Table VIII %Yield-Thermal-tieutron Fission * ield-Fast-Neutron-Fission ~233 ~235 239 238 ~235 ~u239 232 pu T . _ L h 5.78 135 6.03 0.12 6.58 6.59 6.41 0.0065 6.15 6.91 7.17 0.11 6.63 6.3 6.2 6.8 6.3 5.5 6.0

Isotope stable CS133 2.6x106 y 13 d CS136 30 y Cs 137

CS

Cesium-135 is a single f3- emitter and has a long half-life and high fission yield. Its large thermal cross-aectiom (U 3.2 x 106 barns) for

(u-15 barns) and that of its parent Xe135 reduces the cesium-135 concentration long periods of time.

in case of irradiations

The cesium fraction from young mixed fission products has been analyzed for cesium-136 and ce~i=-137 with a multichannel

30

gamma-ray fully

spectrometer. 4.

(31)

T-nis technique

is described

more

in Procedure

A mixture

of cesium-134 cesium

and cesium-137 fraction from a

can generally

be found

in the separated cooled

long irradiated is absent. cesium-133

fuel element,

sufficiently by neutron

so that cesi.um-136 capture by Cesium-134 (45)

The cesium-134

is produced or present

formed by fission has been

as contamination.

in such mixtures Cesium-137 spectra

determined

by gamma-ray

spectrometry. x-ray (4,16)

has been

determined

by means

of the conversion spectrometry.

and by gamma-ray Cesium-137

scintillation

(barium-137m)

has a long half-life, high fission yield,

low neutron and simple

capture decay assay

cross-section (Fig. 1).

(IS<2barns),

scheme of pure

The preferred are 2@(51)

methods

for the routine counter and well-

cesium-137

windowless Several

type scintillation

counter.

methods

for determining

37 7/~+ ~ \\ (11/2-) \

(28.6y) \ 92 ~

Q@- 1.18

BCJi37m 0.662

8 3/2+ Figure 1 -

O/.

IT Ba 37 1 f

Decay

Scheme

of Cesium-137

cesium-137 reported. samples

by gamma-ray (5,49,96]

scintillation

spectrometry rate of pure aliquots,

have been c!esium-137

The disintegration

can be obtai,nedby evaporating Vyns films

free of solids, must ray of be

on gold-coated corrected barium-137

and 41rp- counting.

The counts

for the 10.5% m to determine

conversion

of the 662 kev gamma disintegration

the absolute 31

rate.

Cesium-137

(barium-137m)

liquid

s-dards

are available

fr~ which

Nuclear-Chicago duplicates

Corporation.

They

are prepared

in a rnamer

the methods

previously

used by the National

Bureau

of Standards. Cesium-137 Physical constants has been ueed as a fission concern when monitor. using (16, 17)

are of primary

an isotope Task constants

as a fission Force,

monitor.

The Fuel Burnup

Group,

Dosimetry

A.s.T.M.,

has therefore 6.15% yield

suggested

the following

for cesium-137: fission of U 235

of cesium-137 life,

from thermal-neutron internal ratio conversion

, 28.6 year half

10.5%

of the 662 kev gamma decay. (6) The gamma the presence techniques ting

ray, and 92% branching

for beta

radiation

emitted

by all human describes

beings

indicates and

of cesium-137. to study

Miller(55)

equipnent

developed

the metabolism healthy, human

of gamma body.

ray emit-

elements

in the intact,

VI.

Applications

of RadioisotoPe s of Cesium exhibiting types radiation characteristics testing suitable equip-

Radioisotopes for nuclear ment gages

and other in number,

of nondestructive ones being

are limited

the principal

strontium-90,

thallium-204, The cesium-137

krypton-85, isotope,

cobalt-60, with

cesium-137,

and iridium-192. with

its 510 kev beta is used gages,

in equilibrium gaging

the 662 kev gamma materialp,

of barium-137m and density papers

for beta

of light

reflection There

and radiography. of thickness of betas density

are several either

on the development

gages which and gammas

measure of cesium

the absorption

or scattering A precision

isotopes.

(14,39,73,87)

32

gage

for use under

field conditions

is described density

in the litersgage and a masstrue mass levels (87) flw. (1)

ture. 1) flm meter

A c@bination is utilized

of a cesium-137 in a system

for obtaining
In

A method

to control

large differences of the gamma rays

height

utilizes A gage, soil

the backscattering incorporating densities with

of cesium-137. source,

a cesium-137 an accuracy (12)

gamma-ray of about

can measure

1% and can be used of thickness

at depths gages

down to 1000 feet. include studieB

Other

applications or density

of thickness

preparatory of large

to construcstockpiles of and

tion of highways materials,

and buildings, measurement

inventory

continuous

of the weight uses.

of products,

other process

and quality

control

A gamma milker developed to separate

using

ion exchange

separation

has be,en

the short-lived (66)

barium-137

m fran its longhas many exchangers, flow veloci-

lived parent industrial

cesium-137.

The daughter leakage

product in heat

applications

measuring

flow characteristics ties of liquids. A technique petroleum plant, rivers stocks

of large pipes

or streams,and

to measure

flew rates

of condenser units

water,

circulating water

in and between in open ditches, method

in a refining creeks and (35)

waste

refinery

natural

utilizes Isotopes,

the total-count in order

radiation

of the cesium-134 in industrial reasonably

isotope.

to be useful spectra, at high

radiography, long half-life,

must

have

suitable

and be econcunically produced Cesium-134 has been evaluated

specific

activities.

for use as a .gannnaray source It 1S suitable on the basis

for industrial

radiography.

(19)

33

of gamma activity, able.

radiation but

energy,

satisfactory

half-life,

and specific unaccept-

its cost. per curie makes

it economically

Cesium-137 Dutli with ures using and Taylor those

is a very (20) compare

suitable

gamma

radiographic

source.

its radiographic

characteristics Data on the expos-

of cobalt-60

and 1000 pkv x-rays. of steel,

required

in the radiography and other

iron,

and aluminum (3) steel in

cesium-137 gives

sources

have been when

reported.

Cesium-137

a 2% sensitivity

radiographing (74) curves

the thickness niques

range

of 3/4 to 3 1/2 inches. and sensitivity

Various

tech-

have been

explored of welds

are reported isotopes

for the inspection of thulium-170, A major therapy source

in ship structures cesium-137j

using

iridium-192, medical

and cobalt-60. (72) is in teleteletherapy calibration radiation cobalt-60 of prosources. and

application

of radioactivity a good

devices. because

Cesium-137

is considered makes

its long half-life

repeated favorable used

equipment tection Brucer(g) utilization cesium-137

unnecessary,

and it has more than the more

requirements evaluates

commonly

cesium-137

as such a source.

The design uses of

of teletherapy sources (59)

apparatus

and the medical

are dealt with Recent (10)

in a National

Bureau

of Stand-

ards Handbook. by Brucer

advances

in teletherapy

are reported

and Simon.

Baarli 7) has reported source-skin-distance, using a 50curie

on a plesiotherapy

unit

(short

SSD, as compared source.

to long SSD in teletherapy) for treatment and use

cesium-137

It is useful

of some cancers.

Gauwerky 26) describes

the preparation

34

of cesium-137 application. VII . 1. 2. 3. 4. 5. 6. 7. 8. 9.

applicators

for the treatment

of cancer

by local

Collection

of Detailed Precipitation

Radiochemical - Glendenin - Rider - Lyon

Procedures & Nelson

for Cesium 36 38 39

Perchlorate

(1951)

Chloroplatinate Chlorostannate Tetraphenylboron Bismuth Iodide

Precipitation Precipitation Precipitation Precipitation Precipitation

- Handley - Evans

et al;

(1959)

41 44 46

(1951) (1954) et al. (1958)

Phosphotungstate Treatment

- Mizzan

of Biological Materials Extraction

- Yamagata (1956)

48 50

Tetraphenylboron

- Finston

Thallium (I) Dipicrylaminate Yamagata et al. (1957) Ammonium Perchlorate (1951)

Coprecipitation52 - Glendenin et al. 53

10.

Coprecipitation

11.

Ammonium Cobaltinitrite (1951) Carrier-free Cs 131

Coprecipitation

- Overstreet

et al.55

12. 13.

- Finkle

and Cohn -

(1951)

56

Paper Chromatographic Analysis Crouthsrnel et al. (1951) Anion Anion Exchange Bxchange -Woodhead - Moses

57 (1956) (1959) 59 62

14. 15.

et al.

and cook

35

Procedure

1:

Paper 283 by L. E. Glendenin Perchlorate Method. and C. M. Nelson, Nat. Nuclear Energy Ser., Div. IV, ~, Book 3, 1642-5 (1951). Procedure

step

1.

Add

2 ml of Cs carrier product solution

(ea. 25 rng CSC1)

and 5 ml of 70% tube

HC104 to the fission (note 1). evolve. ethanol, trifuge Evaporate

solution until

in a 50 ml centrifuge white HC104 fumes

dense

Cool the solution and cool and wash

under

tap water,

add 15 ml absolute with stirring. Cen-

the solution 2 times with

for 2 minutes 10 ml absolute

ethanol.

Step

2.

Dissolve boiling

precipitate

in 10 ml H20, heat +3 carrier.

solution

to Fe(OH)3 Centri-

incipient

and add 5 mg Fe of 6 N NH40H

Precipitate (note 2).

by dropwise

addition

with

stirring

fuge and discard of 5 mg Fe 3+

precipitate.

Repeat

precipitation

by addition

carrier.

Centrifuge

and discard

precipitate.

Step

3.

Add 5 drops Add

of 6 M NaOH

and evaporate and evaporate of HC104 ethanol

solution solution

to 5 ml by swirl-

(note 3).

4 ml of 70% HC104 until appearance

ing over a burner under cool tap water,

fumes. with

Cool solution and

add 15 ml absolute

stirring,

for 1-2 minutes.

Step 4.

Filter

precipitate funnel

onto a weighed

filter

paper

(note 4)

in a small ethanol. CSC104, beta

Hirsch

and wash

3 times with weigh

5 ml absolute as

Dry for 10 minutes and meant on a card,

at 11OC, cover,

precipitate

and count with

an end-window

counter.

36

Procedure 1 (Continued)

Notes 1. or Rb In the presence + activities, of K+, NH4+, large amounts of Na+ (?0.5 g)

cesium

can be first separated C88SiW O 12 42 Add

by precipitation

as cesium

silicowolframate,

2 ml Cs carrier tube. Add

and 20 ml 6 M HC1 to the sample 1 ml 0.13 M silicowolframic to stand with solution occasional

in a 50 ml centrifuge H8SlW12042, and allw

acid,

solution

stirring

for 5 minutes.

Centrifuge Dissolve

and wash
h

precipitate

twice with

10 ml 6 M HC1.

precipitate solution boil

1 ml 6 M NaOH

and add 5 ml 70% HC104. to fumes of HC1O dilute 4

Evaporate and then to 10 ml,

by swirling for about

over a burner 2 min.

gently

Cool solution,

and centrifuge. acid. Treat

Discard

the precipitate

of Si and wolframic starting with

supernate in Step

by the regular 1.

procedure

the evaporation

2.

No more

than 5 drops

6 M NH40H

are usually

required.

3.

Raove

traces

of NH: by boiling another

with

NaOH.

Test boil,

for crxnplete and test glass or

r-oval

by adding

1 or 2 drops Store

6 M NaOH,

the vapor with hard rubber

lilmus paper. to keep

6 M NaOH

in waxed

bottle

it free of silica.

4.

Wash

filter-paper

disk with before

ethanol weighing.

and dry under

the con-

ditions

of the procedure

37

Procedure

2:

Report by B. F. Rider, Chloroplatinate Method. Vallicitos Atcmic Laboratory, Pleaaantville, Calif. Procedure

Step H.0,
L

1.

Add

1 ml standardized Fe carrier

Cs carrier (20

m9/ml),

10 ml

5 drops

(10 mg/ml), each)

and one drop each of Ru, Zr, >_.. ___ . (usually 100 A) of

and Ce carriers the fission

(10 mg/ml

to an aliquot

product

solution

in a 50 ml centrifuge

tube.

Step 2.

Add

3 drops

thymolphthalein swirling until

indicator the blue

(0.1% in ethanol) snd point is

and add 1 N NaOH while reached.

Step

3.

Centrifuge

the solution

and decant

the supernatant centrifuge tube.

through

an 11 cm Whatian

#40 paper

into a clean

Step 4. swirl

Add

2 ml 5% chloroplatinic the solution

acid,

H2PtClG.6

H70, water

and to

and heat

in a beaker

of boiling

coagulate

the precipitate.

Step 5.

Centrifuge

solution

and discard

supernatant.

Step

6.

Slurry paper

precipitate

with

H20 onto weighed,

dried

2.4 cm

filter

and wash with water.

step

7.

Dry precipitate weigh

at 135C

for 15 min., on a gamma

cool

in a des-

sicator,

as Cs2PtC16

and count

spectrometer.

Countinq 1. Scan each plate height

Method analyzer. Ccmpare 137 the 660 pre-

on a 256 channel with

kev peak cipitated

of the sample

that of a Cs

standard Small

as Cs2PtC16

and mounted

in the same manner.

38

Procedure 2 (Continued) traces ated of Ru 106 or Zr that are occasionally found are elimin-

in this. manner

(note 1) .

2.

When

Cs134

is present,

it is subtracted

out by complementing a pure

the spectrum

on the 256 channel. analyzer Cs 134 spectrum

and inserting

cyclotron-produced until

in the subtracting Correction

direction can be made

the 0.8 Mev peak cent.

just disappears.

to a few per ~s136

3.

correction cooled

is not usually 60 or more days.

applied

since

samples

have

usually

been

The CS136

decays

to about after is

1/32 in 65 days. irradiation

The spectrum

of a Cs sample

taken

soon

is ccsnplicated, and gamma successful. cs136

ray spectrum

analysis

only partially than Cs137,

yield

is a thousand rates

fold less

so both

are of comparable

decay

at first.

Notes 1. Lacking an analyzer an additional preltiinary CSC104 step is included

in the procedure, Final counting

probably

a preliminary gamma.

precipitation.

is for gross

Procedure

3:

Report Chlorostannate Method. Oak Ridge National Laboratory,

by W. S. Lyon, Oak Ridge, Tennessee.

Procedure Step 1. Add 2 ml standardized 2 ml concentrated Cs carrier HC1, (10 mg CsC1/ml), 1 ml

Fe holdback,

and an aliquot nearly

of the sample

to a 50 ml centrifuge

tube and evaporate 39

to dryness.

Procedure 3 (Continued)

Step

2i

Dissolve

the residue

in 1 ml H20. to boiling.

Add

10ml

1:2 HC1.

C2H50H

and heat

the solution

Step

3.

Add

5 ml boiling and allw

SnC14

(1:2 HC1-C2H50H

saturated

with

SnC14)

reagent

the tube to cool.

Step 4.

Centrifuge with

solution

and discard

the supernatant.

Wash

the precipitate

10 ml 1:2 HC1-C2H50H.

Step 5.

Dissolve

precipitate

by heating

in 3 ml H20. Step 4.

Add

1 ml

Fe holdback

and 5 ml 1:2 HC1-C2H50H.

Repeat

step 6. filter

Slurry

the precipitate in a few ml 4% HC1-C2H50H, and wash with HC1-C.H=OH

L>

on a tared paper,

and ether.

Step m

7.

Dry the sample, CUlture (note 1).

weigh

as Cs2SnC14,

transfer

to a 10 x 75

91ass

tube and count

on a cheater

scintillation

counter

Counting 1. Count the sample on a single

Method channel analyzer 134 set on the and CS136

660 kev peak whjch 2.

to minimize very

contributions

fran Cs

are usually

lcnv. two Cs 137 standards.

Compare

the sample with

Notes 1. Rb+ cm large with amounts

solution

+ of K+ or NH b in the original

interfere 2.

the analysis. accuracy of the methad is believed to be 10%

The over-all

or better. 40

Procedure

4:

Tetraphenylboron Precipitation Method. Paper on Determination of Radioactive Cesium by T.H. Handley and C.L. Burros. Oak Ridge National Laboratory, Oak Ridge, Tennessee. (Anal. Chem. 31, 332-4,-(1959) ) Procedure

Step

1.

Add

1 ml Cs carrier

(ea. 6.5 mg CsCI/ml) to an aliquot

and about

5 mg con-

of Fe, Ba, La, and Zr carriers taining Cs (note 1). just basic Dilute

of the sample

the solution

to 15 ml and add 1 M dd 1 1 3 M a2c03 Centrifuge

NaOH until and warm

to phenolphthalein. to coagulate

the solution

the precipitate.

and discard

precipitate.

Step

2.

Make

supernate

just acid with Repeat

6 M HC1 and add 5 mg each hydroxide and carbonate

of Fe, Ba, La, and Zr carriers. precipitation. Step 3. bath. Make supernate

just acid with stirring

1 M HC1 and cool

in an ice (note 2)

Add dropwise solution

while

1 ml of Na@4B

solution

and allw

to stand

for 10 minutes. with

Centrifuge 5 ml H20,

solution centri-

and discard

supernate. wash

Wash precipitate solution.

fuge and discard

Step 4.

Dissolve

precipitate solution solution solution

in a minimum

of acetone

and add 1 Add

ml 1 N HC1. dropwise minutes. precipitate

Dilute

to 10 ml with water and allow solution

and cool. to stand

4 ml Na@4B Centrifuge

for 10 Wash

and discard

supernatant.

with water

and discard

supernatant.

-
1
ml;

Dissolve

precipitate

in a m$nimum alcohol

of acetone,

usually of

add 10 ml of absolute and cool the solution

containing

0.5% by weight with

Na@4B

in an ice bath

for 10 minutes

41

Procedure 4 (Continued) occasional Whatman stirring. Filter precipitate disk onto a tared NO. 42 and waeh with at 11OC several

or a Munktell

No. 00 filter

small portions minutes beta

of alcohol. as a Cs@4B

Dry precipitate (note 3) .

for 15 for

and weigh

Mount

precipitate

counting

or place

in a suitable

tube for gamma

counting.

Countinq 1. In old mixed present. previously samples 137 fiesion Count products cesium

Method
1-47

CsA

is the only cesium type scintillation

radio-

nuclide counter 2. Cs

in a well with a CS

calibrated from yo-mg

137 standard. that. contain Deter-

Count 136

mixed

fission products gamma-ray

and Cs

on a multichannel

spectraneter.

mine

Cs13 by integration of Canpton assume Cs 137

of the 1.04 Mev photopeak

following

subtraction

distribution that Cs 136

frmn the 1.25 Mev photopeak. decays 100% through the 1.04 Mev photopeak 1.25, thesarne Compton

For calculation gaimna. Determine

by integration

of the 0.662Mev frmthe

following 1.04, energy

subtraction

of the Ccdnpton distribution Count radionuclides to establish

and 0.82 Mev gammas. under identical

of nearly the correct

conditions

distribution

for subtraction

from the spectrum of Mn 54 .

of the unknown. For the 1.04 Mev 22 . A factor of

For the 0.82 Mev peak use a standard peak use Zn 65

and for the 1.25 Mev peak use Na for calculating correction gamma

0.82 was used This factor

the disintegration for branching of cs

rate

137 of Cs . con-

includes

and internal

version gration

of the 0.662 wv rate use is made

137. . To obtain the disinteas a function

of photopeak-to-total-ratio

42

Procedure 4 (Continued) of gamma-ray energy and source radionuclide distance. (1,2) The disintegration

rate of a specific relationship:

is given by the follclwing

Disintegration

ND P Rate . EtPABY

NP Dt PA-

integrated dilution

area under photopeak factor for source

total absolute detection efficiency detector geometry used appropriate value for peak-to-total

katio and

correction factor any beta absorber correction conversion chemical

for absorption in source used in measurement

B-

for branching ratio and internal of the gamma measured

Y-

yield.

1.

In the presence Cs carrier, (1 g/ml)

of macro
15 ml

amounts

of Rb and K, add 1 ml standacid,

ardized

6 M HC1, and 2 ml silicotungstic

8siw12042, Digest natant.

to an aliquot

in a 50 ml centri:Euge tube. centrifuge, and discard super-

the sample

for 10 minutes, with

Wash precipitate

5 ml 6 M HC1.

issolfe cs8siw12042 add 20 ml

precipitate

in 1/2 ml 6 M NaOH yellow

(warm, if necessary); Add

6 M HC1 and discard Digest Wash 1) 2) sample

precipitate. centrifuge,

2 ml H8SiW12042. supernatant. in 1/2

for 10 minutes, with

and discard

precipitate

5 ml 6 M HC1.

Dissolve

precipitate

Heath, Bell,

R.L.$ P.R.,

IDO DaViS,

16408, R.C.,

(July 1957) Lazar, 43 N.H.3 ORNL Rept. - 72 (1957)

Procedure 4 (Continued) ml 6 M NaOH. addition 2. Begin

step 1 of regular

procedure,

omitting

the

of Cs carrier. Na@4B solution by dissolving 4 g Na@4B and 1 g indiis just and it

Prepare

AlC136 cator

H20 in 100 ml H20. Add

Add a few drops until

phenolphthalein the solution filter, where

solution. Allow

6 M NaOH dropwise

alkaline. dilute will 3.

solution Store

to stiand several solution

hours,

to 200 ml.

in a refrigerator

keep

for several yield

months. is usually 75% or better. A decontamination tested and for

The chemical

factor mixed

> 106 wag obtained fission product

for eack radion~clide

solutions.

Procedure

5:

Bismuth Iodide Method for the Determination of Paper 284 by H.B. Cesium Activity in Fission. Evans, Nat. Nuclear Energy Ser., Div. IV, ~ Book 3, 1646-8 (1951). Procedure

Step

1.

Add

20 mg standardized

Cs carrier

(1.263 g CsC1/100

ml

in H20 standardized carrier

by chloroplatinate

methodl) , 20 mg Rb 5 mg each of Ce, Y, La, of fission material

(1.414 g l?bc1/100 ml in H20),

Zr, Ba, and Sr carriers

(note 2]. phthalein Add 12 N NaOH

(note 1) to the sample until the solution

is basic

to phenol-

and then

1 ml 1 M Na2C03.

Centrifuge

and discard

preci~itate.

Scott, W.w., Standard Methods of Chemical Analysis, vol. 1, p. 869, D. Van Nostrand Co., Inc.

5th Ed.,

Procedure 5 (Continued)

step

2.

Acidify

supernatant

solution

with

concentrated HC1, add to make solution

about basic

10 mg La carrier, to phenolphthalein.

and then add 12 N NaOH Centrifuge

and discard

precipitate.

Make

supernatant

solution

acid wikh

glacial

HC2H302 Cool for

(note 3) and then add 1 ml HI-BiI s reagent several minutes (note 5) and centrifuge.

(note 4). Supernatant

solution

can be used

for Rb analysis.

Step 4. solution

Wash precipitate cool. Centrifuge

with

7 ml H20 and 1 ml

2 M HC1, keeping in 6 drops and 1 ml several

and dissolve Add

precipitate

cone. HC1 by heating

to boiling.

10 mg Rb carrier Allow

H*O .

Cool and add 1 ml HI-Bi13 and centrifuge.

mixture.

to stand

minutes

step

5.

Wash precipitate disk,

with

cold

2 M HC1, with

filter

onto weighed

filter-paper absolute weigh as

and wash

successively

5 ml F)ortions of

ethanol cs3Bi219

and ether. (note 6).

Dry at 11OC.

ior 10 mi,nutes and

Notes 1. Sample may contain either U or Pu as either nitrate or

chloride cipitation 20

(sulfate removes

solutions bulk

have not been

tested).

First pre-

of the U or Pu. aids in removal of fission-product

Addition

of these

carriers

cations. 3. If the volume exceeds 15 ml, it is best to evapcmate the

solution

to this volume.

Procedure 5 (Continued)

4.

The HI-Bi13

is prepared of some

by dissolving free iodine

10 g Bi13

in 50 ml with

55% HI.

Presence

does not interfere

the precipitation. 5. Precipitate of CS3B1219 fozmm quite rapidly and is very

insoluble 6.

in cold dilute

HC1 or HC2H302. f&m other fission elements ia

If greater

decontamination

desired,

the CS3B1219

is dissolved

and the Csis schme: h

reprecipitated issO1ve CS3B1219

as CsfiPtC16 according * precipitate BoI1

to the follcndng

frcm step 5 of above procedure 12, add 1 ml cone. HNO 3 and

about

2 ml 6 M HN03. cOO1

to remove

3 1 2 d

the solution. should Wash remain

To the cool solution cool), with

add 10 ml ethanol

(solution alcohol.

0.5 ml 0.5 M H2PtC16, filter onto

and 7 ml more

Cs2PtC16

alcohol,

filter-paper dry at 11OC.

disk of and weigh

Whabnqn

No. 50 paper, . provides

wash with

ether,

as Cs PtCl 26 7. Method

a decontamination

factor

>10

fran other a decon-

fission

activities factor

if Cs is reprecipitated >105

aa Cs3Bi219;

tamination

if Cs is reprecipitated

as Cs2PtC16.

Procedure

6:

Phosphotungstate Precipitation Method of Analysis of Radioactive Cesium in Solutions of Long-Lived Fission Product Activities by E. Mlzzan, Chalk River Atomic Energy of Canada Limited (PDB-128) (1954). Procedure

Step 1. fission

Pipette product

aliquot activities

of aqueous into a 12

Bolution
ml

of the long-lived tube containing

centrifuge

Procedure 6 (Continued) 6 drops carrier CB carrier . (12.7 g CaCl . (20.5 g RuC13 h 1 liter H20),, 1 *OP ~d 0.5ml ,. (29.4 g Z:O(N03)2~20 in 1 liter H2@, ,, Ru

in 1 liter H20),

Zr carrier, .,

Step 1 ~

2.

Dilute

8-10 ml with

5 N IiIJ03 and add with atlrrtig (66.2 gP205~24,wo325H20 in. ,.

0.05 Hphoaphotungstate 1).

acid

400 ml H20) (note

Step

3.

Let stand

5-10 minutes,

centrifuge,

and diecard

a@er-

natant.

step 4.

Waah

precipitate

thoroughly auparnatant..

with

8-10 ml 5 N HN03,

centrifuge,

and discard

step 5.

ReXat

Step 4.

Step 6. pleteiy

Slurry by -a

precipitate

with

34

drops

H20 ,ti

tranafer

ccnn-

of a, apitzer

onto

an aluminum

disc. ofH20

Rin~e, aplace

centrifuge

tube aI@

q pltzer with timall portions

on the disc.

step 7.

Dry precipitate

underan

infra-red

lamp.

step 8.

Dry precipitate @ote .2).

further

on Pul-control

heater for about

30 aeconda

Step

9.

Cc&k with .,..,,

a G.M.

end-window Hotea .,,

counter

(note 3)j

..

1.

Waah

atirri.ngrod repwing

free

of

any .precipitate tube..

by fine, stieaq. of

water

before

fran centrifuge

47

Procedure 6 (Continued) 2. Heat precipitate - about at full heat until orange-yellow coloration

appears 3.

30 seconds. yield, self-absorption is canplete and self-scattering and the amount of and

NO radiochemical

are required. inactive

The Cs recovery

Cs carrier

is so chosen cancel

that the seif-scattering

self-absorption 4. ties

effects

each other. long-lived fission product activi-

Ikcontamination is satisfactory.

fran other

Procedure

7:

Separation of Radioactive Ceaium in Biological Materials. Paper by Noboru Yama9ata and Toshiko Yamagata (Bull. Chem. Sot. Japan, vol. ~ No. 9, p. 1063, 1958),

Procedure l Salnpe Prep&ratitin 1. Urine - add 50 ml HW03 in a beaker and 2 ml cs carrier and evaporate (CSC1-1O mg Cs/ml) Transfer with to

to 500 ml urine a porcelain HN03 mixture times

to 50 ml.

dish and heat

to dryness. to dryness. matter.

Moisten Repeat

residue

HCl-

(1:1) and heat all organic hotwater

treabnent

several with

to deetroy

Extract

dried

residue

five 50 ml portions to approximately

and filter.

Bring

ccmbined

filtrate

300 ml and follm

separation

procedure.

2.

Cereals,

Vegetables, g dried

and Dry Milk vegetables,

- dry ash about 50 g dry milk) with

300-500

cereals Extract

(100-200

at 400-450c. five 50 ml

ashafter addition

of 2 ml Cs carrier

48

Procedure 7 (Continued) portions hot HC1 (1:10] and filter. Transfer mmbin,ed adding filtrate 50 ml

to porcelain HN03 .

dish and evaporate dried residue

to dryness

after

Extract

with

five 50 ml portions to approximately

hot water 300 ml and

and filter. follow

Bring

combined procedure.

filtrate

separation

3.

Soil

(N-ammonium solution

acetate

extraction)

- add 3 liters

N-ammonium

acetate

(PH 7) to 300 g fresh occasional

soil in 5 liter beaker. and filter. dish Add to dryRepeat

Let stand 4-5 days with 2 ml Cs carrier ness. several residue combined procedure Moisten times with

agitation

and evaporate residue

filtrate

in porcelain

with HC1

(1:1) and heat matter.

to dryness. Extract dried

to destroy

all organic

five 50 ml portions to approximately

hot water

and filter.

Bring

filtrate .

300 ml and followr separation

separation 1. Add NH40H dropwise until dense Allow precipitate to settle of ph~osphates and test supernatant .Fi.lterand wash and washings

appears

and add 2 ml excess. precipitation with NH40H precipitate.

for complete precipitate and discard

by addition

of NH40H. filtrate

(1:100).

Combine

2. Add

Add

20 ml HN03 and 5 mg J? (as H3P04) agitate

and heat

tc> 50-60c. and rub and

20 ml 10?4 (NH4)6 M07024 4H20, a glass rod to hasten

vigorously,

wall with cool . yellow

precipitation. HN03

Let settle

Filter

and wash with with

5 portions

(2:100).,

Take up Boil

precipitate

NH40H

(1:1) and wash with water. 49

Procedure 7 (Continued) canbined Dilute filtrate and washings until odor of ammonia. disappears.

to 100 ml and cool.

3.

Add

1 ml ho% H2PtC166H20 yellow precipitate

with

stirring.

Rub wall with several

glass

rod until Filter

appears.

Let stand

hours.

through with

weighed

one inch filter paper and 3 portions

in Hirsch ethyl

funnel Dry

and wash at 11OC with

10 ml cold water Mount 137

alcohol. counter

and weigh.

for counting.

Standardize

kncnvn amount

of Cs

and 20 mg Cs carrier

precipitated

as

chloroplatinate.

Notes 1. Overall yield of Cs is >85% is >105 of ma ~~137 and decontamination and Sr8. small in the counting. fran other

fission 2.

activities
L

for Ce144

Contribution of

and ~40

is negligibly materials

determination

in biological

by beta

Procedure

8:

Tetraphenylboron Extraction Method. Report by H. L. Flnston, et al., Radiochemical Analytical Section, Brookhaven National Laboratory, Upton,

N.Y.

Procedure Step 1. Pipette ad an aliquot of the fission product solution in 0.5 M HN03 volume to 15 ml

(~ 5 ml)

10 ml buffer

solution

11 M Na3C6H507 Adjust

pH = 6) into a 125 ml separator with H20.

funnel.

Step

2.

Add

an equal

volume

of 0.05 M Na@4B

amyl

acetate

and

50

Procedure 8 (Continued) extract the Cs activity 30 sec. into the organic phase by shaking for

approximately

Step

3.

Transfer Step 2.

aqueous

phase

to another phases

separator

funnel separator

and

repeat funnel.

Cmbine

organic

in the first

step with

4.
tWO

Strip

Cs activity

from the amyl acetate 3 N HC1.

phase

by washing

successive

10 ml portions

Step 5. Steps

Evaporate 4.

acid

solution

nearly

to dryness

and repeat

1 through

Step 6. aliquots

Dilute

aqueous

phase

to krmvn

volume

and take counter

suitable (note 3) .

for counttig

in a y-well

scintillation

Notes 1. 2.
is ~

Time Yield

for separation

in duplicate

is approx~tely factor from

30 minutes. fission products

is 100% and decontamination Although valid procedure was

106.

developed containing

for tracer

solutions

it has proved carrier.

for solutions

up to 10 mg Cs

136 Ad 3. Cs The well 137 counter is calibrated When for efficiencies of Cs is amounts

vs. a 41r@- count.

the history

of the sample

known

(i.e. the irradiation isotope

and decay

times)

the relative

of each

are calculated.

51

Procedure

9:

Thallium (I) Dipicrylaminate Precipitation Method. Paper on Carrier-free Separation of Cesium from Fission Products by the Use of Coprecipitation with Thallium (I) Dipicrylaminate by Noboru Yamagata and Sadakata Watanabe (Bull. of the Chem. Sot. of Japan ~ NO. 6, p. 580, 1957). Procedure

Step

1.

Add

20 mg Fe

(Fe(N03)3 product

solution) solution

and 5 mg Sr (note 1) .

(Sr(N03)2 Make basic

solution) to thymol Filter Step 2.

to the fission blue

(pH 8-9) with precipitate

NaoH

solution,

and add 1 ml I.M NaCo3.

and was

with water. if necessary, 1 and cool with to pH 8-9, add lCMI% for half hour constant In ice

Neutralize 3% sodium Add

filtrate,

excess water.

dipicrylaminate,

1 ml 0.1 N T1N03

dropwise Filter

stirring, and wash ether

and stir for 30 minutes with 2 ml, ice water

at OC.

precipitate

and with

two 2 ml portions of diethyl

at OC.

Step

3.

Take precipitate funnel. Shake

up in 5-10 ml methylisobutyl Add 1 ml saturated chlorine

ketone water and

in a separator 5-10 ml aqueous Step 4. aqueous layer 2N HC1. layer Add

vigorously separator

for 1 minute funnel.

and transfer

to another an equal Shake

volume

of methylisobutyl for 1 minute. dish

ketone

to the aqueous

layer.

vigorously

Evaporate

to dryness

in a small

counting Notes

and count.

1.

Sample

must

not contain

K, NH4,

or Rb since solids

they will

be

present 1

in the final product

as inert

and are remwed of Metalsn,

E.B. Sandell, Colortietric Determination of Traces InterScience Pub. Inc., N.Y. (1950), p. 501.

Procedure 9 (Continued) difficulty. If U is present removed in the fission product sample,

With

it must be previously 2. The recovery factor

by solvent

extraction. deconis

of active is >10 4

Cs Is about

90% and the groaa procedure

lamination valid only

, although

the proposed

for about

one year

old fission

products.

Procedure

10:

Preparation of Carrier-free Cesium Tracer by Use Paper 285 by L. E. Glenaenin of Ammonium Carrier. and C. M. Nelson, Nat. Nuclear Energy Ser., Div. IV, ~, Book 3, 1649-51 (1951).

Procedure Step 1. Add 1 ml 1 M NH4C1 and 5 ml 70% HC1CY4 to the sample tube. fumes under of

fission

material

(note 1) in a 50 ml centrifuge until dense white

Evaporate evolve running

by swirling (wear safety tap water

over a burner glasses).

HC104

Caution:

cool the solution ethanolt

(note 2) and add 15 ml absolute Centrifuge and wash

cool and stir twice with 10

for 1-2 minutes. ml absolute

precipitate

ethanol.

Step

2.

Take up precipitate i-!+ carrier.

in 10 ml H20, heat Add 6 M NH40H

nearly

to boiling, stirring, and

and add 5 mg Fe until Fe(OH)3

dropwise

with

precipitate Add

coagulates another

(note 3) . *+

Centrifuge

discard

precipitate.

5 mg Fe

. carrier,

centrifuge,

and discard

precipitate.

Step

3.

Evaporate

supernatant

solution

to about

5 ml,

add 4 ml

70% HC104,

and evaporate

to HC104 53

fumes by swirling

over a burner.

Procedure 10 (Continued) Caution: absolute ethanol. cool under ethanol. running tap water (note 2) and add 15 ml 10 ml absolute

Wash precipitate

twice with

Step 4. dryness.

Add

5 ml aqua regia

to precipitate

and evaporate

to

Step

5.

Repeat

Step 4 tWiCe.

Step 6. H20.

Take up carrier-free

Ca activity

in suitable

volume

of

Notes 1. Original sample must solids not contain K or Na, since they will be

present 2.

as inert

in the final product. conditions ethanol when of the procedure, to HC104. ethyl perThis canpound

Under

the anhydrous is formed when explosive and after

chlorate is

la added

extremely

heated.

The solution of ethanol,

must be kept

cool during solution 3. 4.

the addition

and the aupernatant

should

be discarded

at once. is usually required. in water solu-

No more Final

than 5 drops

6 M NH40H

product a small

la free of solids amount of HC104.

and is present

tion with

9+

Procedure

11:

Note on Preparation of tirrier-free Cesium Tracer. Paper 286 by R. 0ver8treet and L. Jacobson, Blat. Nuclear Energy Ser., Div. IV, ~, Book 3, .1652-3 (1951) . Procedure

Step 1.

Digest

an alkaline products

NH20H

filtrate

frcnn a large 5 g U, Sr

sample 09 ,Ba,

of

unseparated ~140 , Ce 137

fis~ion

containing 106

about

140

, and traces

of Ru

and Te12

with

aqua regla

to

destroy Remove

NH20H.

Add 50 mg CUC12

and adjust

acidity

to 0.5 N HC1.

Cu and traces

of Ru and Te as the sulfides.

Step Add

2.

Bring

filtrate

to pH 2.5 and precipitate and then remove wittaqua with

U04 with

H202.

Sr and Ba carriers

(NE4)2C03.

Destroy

the lrH4Cl in the filtrate

regia.

step NH4Cl

3.

Evaporate

residue

and take up in 1 N HC2H302. to precipitate theNH~

Add

50 mg

and sodium

cobaltinitrite

and CS137

tracer.

step 4.

Decanpose~ecipitate

in aqua regia carriers.

and add Sr, Y, Zr, Add 50 mg ~4cl and

Ru,

Te, Ba, La, ce, and Th holdback reprecipitate NH: with sodium

cobaltinitrite.

step 5.

Decanpose

precipitate

again

and make

a third precipita-

tion without

addition

of holdback

carriers.

Step

6.

Decanpose

precipitate

agati

and rmove

Co as COS at pH 8-9.

Step

7.

Evaporate

filtrate, Adjust

decaupose solution

~4Cl,

and convert

residue to

to the chloride. other preparations.

final

to pH 2.6 to conform

55

Procedure

11 (Continued)

Notes 1. Assay shws that the radioactive and that no detectable contamination quantities of the cesium of inert hold-

sample back

is <0.5%

carriers

are present.

Procedure

12:

c~131 Tracer. Preparation of Carrier-free 10 d Paper 207 by B. Finkle and W. E. Cohn, Nat. Nuclear Energy Ser., Div. IV, ~, Book 3, 1654-6, ~ (1951).

Procedure Step 1. Irradiate a quantity of ignited Bakers BaC122H20. the Ba salt in six

days after

the end of the irradiation, to volume with H20.

dissolve

3 N HC1 and dilute

8tep

2.

Precipitate 3 N HC1.

BaC03

WI-

(NH4)2m3

and dissolve with cone. HC1.

in minimum

amount

Precipitate

BaC120H20

step

3.

Dissolve

in H20 and reprecipitate

BaC12.H20

three

times.

step 4.

Dissolve ,

BaC12,

dilute

with

H20, and scavenge ,,.

with

Fe++

precipitated

with NH40H.

Step 5. BaC12

Scavenge

supernatant This

with gives

La(OH)3

and make

two more

precipitation.

a clean Ba source. 131

Step

6.

After

several

days milk

Ba

of its cesium BaC12=H20

daughter

by

dissolving

Bac12

in H20 and reprecipitate

by drapwise

56

Procedure

12 (Continued)

addition of cone. aside for future

HC1 with Cs 131

vigorous

stirring.

Set precipitate

production.

step BaC12

7.

Clean

supernatant

8olution

of all Ba activity addition,

by five with

precipitations,

carried

out by dropwiae

stirring,

of 1 ml inactive

Ba carrier

(15 mg/ml).

Step

8.

Boil

supernatant twice with

5

solution
mg

to dryness,

dissolve

in H20, of

and scavenge reagents.

La(OH)3,

with mintium

amount

Step 9.

Evaporate

tracer

Bolution

to dryness leaving

several solid-free

tLes

with

aqua regia ~131

to remove

anmonium

salts,

10.2 d

activity.

Notes i. The product

iB abOUt

has high
30%.

radloch-ical

purity,

and the overall

yield

Procedure

13:

Paper Chranatographic Analysis of Irradiated Uraniti in a Hydrofluoric Acid Medium. Paper by C. E. Crouthamel and A. J. Fudge. J. Inorg. Nucl. chin. ~, 240-244 (1958) and Quantitative Determination of Fission and Nuclear Reaction Products by C. E, Crouthemel, R. Heinrich, and C. Gatrc)uses, Talanta ~ 396-407 (1958).

Euuipment 1. Papers No. used were 2 paper 1/2 wide strips. Whatman 3-MM, Whatman were No. 1, or

Whahan

The papers

not pretreated.

57

Procedure

13 (Continued)

2.

Experiments centered

were

run in closed

polythene

cylinders

with

the

paper

at the top by a split cork was centered to the plane the paper solution was

stopper..

At the bottcm spltie placing

of the strip inserted

the paper

by a flat platinum of the paper in position, before

perpendicular men

in the cylinder. below

the spline was sample of the

the developing about

surface,

and the original

spot was polythene

2.0 cm above

the surface. Smallc boundary

The free volume

cylinders

was relatively the solvent was

29 rmn diam. by 30 cm. was visible with through vapors a

With proper

lighting,

the polythene. by wetting strip

The atmosphere with

saturated

solvent

the walls

the solvent

just before

fitroducing

into the vessel.

Procedure Step 1. taining Dissolve about irradiated uranium oxide with cone. HNO
3 con-

1 pg Cs carrier

per u l in a platinum crucible.

Step under

2.

Evaporate

to dryness

with

a small

amount HF.

of cone.

HnTO 3

an infra-red

lamp and dissolve

in cone.

Step

3.

Convert cone.

nitrates

to fluorides

by two successive h 1:3 HF.

evapora-

tions with

HF and dissolve

residue

Step 4.

Place

2-100 l.lg uranium strips

Solution

in a 5-10 mm circle to spread to

on Whabnan

paper

and air dry.

130 not allm

edge of the paper.

Step 5.

Place

paper

strip

in the polythene

cylinder

and develop

Procedure

13 (Continued)

with

60 g 49% HF per 100 ml dry CH C H CO. 325 to develop.

Chromatograms require

3-5 hours

step with

6.

Cs isotopes counter

were

detected

at center with

of chrcnnat~ram slit over

a Geiger

probe

equipped

a defining

the window

(note 1).

Step 7.

Cut paper

and mount

between

25 mil mylar

plastic

and

count with

a scintillation

spectrometer.

step 8.

Obtain

absolute

disintegration peak

rate by canparing

count-

ing rate under calibrated Cs

662 kev gamma

of the sample

and a 47r~-

137

solution

chrmatographed

in the same manner.

Notes 1. 2. The yield Method of Cs by this analysis is 100%. of very low burn-up

is not applicable a large

to samples amount

values

that require

of fissile

fuel.

Procedure

14:

The Rapid Determination of Radioactivity Due to Cesium-137 in Mixed Fission Products by Anion Exchange and Gamma-Ray Spectrcmetry. Report by J. L. Woodhead, A. J. Fudge, and E. N. Jenkins, United Kingdan Atomic Energy Authority, AERE C/R 1877, Feb. 23, 1956.

Preparation at 11OC. Make

of Resin Zrind

- Dry normal mill

grade

Deacidite

FF for 16 hours size.

in a coffee

and grade

into 80-100 mesh and

into a column,

12 x l, by pouring

into H20 slowly

59

Procedure

14 (Continued)

allowing about

to settle

otit.

Pour

3 M Na2C03 volumes volumes

through (~250 (z500 bottle

the resin

at

10 ml/min

until

10 column

ml) have passed ml) of demin-

through. eralized

wash with water.

twenty resin

column

Pour

into stoppered

and store under

demineralized

H20.

Procedure Step 1. form, a well Slurry 1 g Deacidite column, FF (80-100 mesh), in the carbonate fitted with at top

into a glass ground

25 cm x 0.7 cm diameter, Use cotton

tap and a fine tip.

wool plugs

and bottcm

of the resin bed.

Step

20

Drati wool

the water pad

frcm the column

until

just above

the

top cotton

(note 1).

Step

3.

Take an aliquot

of fission

product

solution

and adjust with

its acidity H20

to pH 1 by addition

of alkali

or by dilution

(note 2).

Step 4. Zr

Add

0.1 ml aliquots

Cs

(7.33 g CsN03/103 ml) and Ba solution

ml),

Ru

(note 3),

(3.0 g ZrN03

+ 1.0 g H2C203/100 product

(1.9 9 Ba(N03)2/100 and add 1 ml of the

ml) carriers mixtureto

to the fission column.

the resin

Step 5. collect

Allow

fission

product

solution

to run into resin

and

eluant. at about Wash column

6 drops/rein (0.3 ml/min) with 4 ml demineralized

in a small polyH20 and collect

thene cup. in same cup.

60

Procedure

14 (Continued)

step

6.

Stir

the solution

with

a thin polythene on the Al housing spectraneter.

rod.

stand

the

cup ,on a 250 rng/cm2 Al absorber crystal of a ganma scintillation

of a NaI(Tl)

EQ3Lz
solution

Determine

the peak height cup under

of 5 ml of a 4T@gemetry.

counted

Cs

137

in a similar

identical

Notes 1. care must be taken never to allow the colk to run dry at

any time during 2.

the procedure. must not be greater than 3 M in the

Salt concentration prepared

finally 3.

sample. RuC13
in an alkalihe

DiSSOIVe

2.04 g specpure with

solution

of

K104 . with

Stir solution

an equal Wash

volume

of CC14

and make

acid and frmn

concentrated

H2S04.

CC14 phase

once with water nitrous fumes

treat with action

30 ml B M HNQ3.

Gas mixture until

with

of 8 M HN03 solution

on Cu turnings to remove H20.

no more

Ru is extracted. cool, and

Boil HN03 dilute

excess

nitrous

fumes,

to 100 ml with

61

Procedure

15:

Radiochemical end Mares Spectraneter Studie8 of Fit3Bion Product Cesium. Report by A= J. :Mdtiea. ., and H. D. Cook, Analytical ChaUiatry in lEuclear Reactor Technology, Second Conference; Gatlhburg, : Tennessee, TID-7566(Pt.2), 192 (April 1959). of The Rapid Determination of Radioactivity DUS to CeEIium-137 in Mixed Fission Products by Anion -change and Garmna-Ray Spectranetry byJ. L. W60dhead, A. J? Fudge, and E. N. Jenkins, United KingdanAtanic ~ergy Authority, AERE C/R 1877, Feb. 23, 1956;

Nodificaticm

Procedtie Stem 1. fid am aliqiot of the mixed reein fission product solutim
forh

to at a

a Dm?~-1

anion-exchange (note 1).

column in the carbonate

pH of about6

step

2,

cesium wiih

elutes

in the first

3 ml.

The column

is then

washed

5 ml H20.

Step apply

3.

Etnne eiuate

to dryneaa

with

H2S04, emission

contiti mass

to chloride,

to source

filament

of themal

spectrmter

for isotopic

analysis.

Motes

1.

Resin

serves

as a solid precipitant

for precipitating

Zr,

Nb, RU end Ce. 2. Recovery of carri&-free Cs fraction. . Cs is nearly 10W: ganma spectraaetry

indicates

pure

62

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1) Aebersold, P.C. and Fowler, E.E., Proc. U. N. Intern. Conf. Energy, 2nd, ~ P/1794, pp. 76-83 (1958). Peaceful Usee Atmic Spectrochemical Ahrens, L.H., Quantitative Silicates, pp. 47-73, Addison-Wesley Pub. 42, Mass., (1955). Anderson, M.B., J. Sot. Non-Destructive pp. 365-70 (1959). Aoki, F., Kurosawa, pp. 5B3-5 (1957). T., Yajima, Analysis of Co., Inc., Cambridge

2)

3)

Testing

XVII,

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4)

S., Bull.

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Aoki, F., Yajtia, S., Kurosawa, pp. 42-45 (1959). ASTM, Communication (Dec. 1960).

T., Bull.

Chem.

Sot. Japan ~

6)

from Committee

E-10,

Fuel Burn-Up

Group,

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Baarli, J., Prog. in Nuclear Energy, pp. 229-40, Pergamon Press, New York Brooksbank, pp. 819-23 W.A. and Leddicotte, (1953).

Series VII, (1959). J. Phys.

Vol.

2,

8)

G.W.,

Chem. ~

9)

Brucer, M., Proc. Intern. P/179, pp. 68-74 (1956).

Conf. Peaceful

uses Atomic

Energy

10,

10)

Brucer, M. and Simon, N., Prog. in Nuclear Energy, Series Vol. 2, pp. 209-15, Pergarnon Press, New York (1959). Caley, E.R. and Deebel, W.H., Anal. Chem. 33, pp. J. Appl. 309-10 Radiation

VII,

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12)

Caineron, J.F. and Bourne, M.S., Intern. and 160topes ~ pp. 15-19 (1958). Cohn, W.E. and Kohn, H.W., J. Am. Chem.

13) 14)

Sot. ~,

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(1948). Energy

Crcanpton, C.E., Proc. 15, P/164, pp. 124-34

Intern. Conf. (1956).

Peaceful

Uses Atomic

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Crouthame 1, C.E. and Fudge,

pp. 240-4 (1958).

A. J., J. Inorg.

Nuclear

them. ~,

16)

Crouthamel, pp. 396-407 Crouthamel, uses Atanic

C. E., Helnrich, (1958).

R., Gatrousis,

c. , Talanta

l-, No. 4,

17)

C.E., and Turk, E., Proc. Energy ~, p. 27 (1956) . G.A., -al.

Intern.

Conf.

Peaceful

18)

Dallon, J.C. and Welch, (1956) .

Chim. Acts 15, pp.

317-19

19)

Dutli, J.W. and Elliott, D.E., ~, No. 2, pp. 24-7 (1956). Dutli, J.W. and Taylor, C.M., ~, NO. 2, pp. 35-8 (1954). Dutt, N.K., J. Indian Chem. C@n.

J. Sot. Non-Destructive

Testing

20)

J. Sot. Non-Destructive

Teeting

21) 22) 23)

Sot. ~

pp. 71-4

(1945). (1938). Section

Feldman, Finston, (1956) .

R.V., H.L.,

J. Appl. B.N.L.

(USSR) ~

1017-22

Report,

Radiochemical

Analytical

24)

Freiling, E.C., Pascual, pp. 330-1 (1959). Furman, N.H., 5th Ed., vol. (1939) .

J., Delucchi,

A.A.,

Anal.

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COMMITTEE

ON NUCLEAR

SCIENCE

John Huizenga, Chairman, Nuclear Strutiure Thomas A. Tombrello, C. K. Reed,

Rewarch Laboratory

$ice C/rairrnan, California institute off Technology Academy of Sciences

Executire Secretary, National

Lowell M. Bollinger, Argonne National Laboratory Peggy Dyer, University of Washington Russell Heath, Aerojet Nuclear Co., inc. Roy K. Midd!eton, University of Pennsylvania a

1. Lon Morgan, Columbia Scientific Industries G. Davis OKelley, Oak Ridge Netional Laboratory G. C. Phillips, Rice University Henry N. Wagner, Jr., The Johns Hopkins Medical Institutions Joseph Wenaser, Brookhaven National Laboratory Sheldon Wolff, University of California Chien-Shiung Wu, Columbia University Alexander Zucker, Oak Ridge National Laboratory

Liaisonembers M
William S. Rodney, National Science Foundation George L. Rogosa, Enargy Research and Development Administration

SUBCOMMITTEE

ON RADIOCHEMISTRY

G. Oavis OKeiley, Chairmerr, Oak Ridge National Laboratory Glen E. Gordon, University of MaryIand Rolfe H. Herber, Rutgers University John A. Miskel,
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Jr., Los Alamos Scientific Laboratory

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Liaisonembers M
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