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PREFACE

This report i s an evaluation of a l i t e r a t u r e survey t h a t w a s under-

taken at t h e request of t h e Division of Reactor Development and Techno-

logy, USAEC, t o ascer ta in t h e e f f e c t of atmospheric contamination during

sample handling on t h e ana lys i s of a l k a l i metals. Information w a s

s o l i c i t e d from those chemists and meta l lurg is t s who are a c t i v e l y engaged

i n a l k a l i metal analysis . While no attempt w a s made t o associate any of

t h e comments i n t h i s report with any p a r t i c u l a r individual or with any of

the l i t e r a r y references which appear as a bibliography i n t h e Appendix,

a l l conclusions are based on the experiences of t h e author as wel l as on

t h e conpnents of those of t h e individuals surveyed or on those references

appearing i n the l i t e r a t u r e . We wish t o express our appreciation t o t h e

following individuals who cooperated so w i l l i n g l y e i t h e r by supplying

information based on personal experiences or by suggesting references

i n t h e open l i t e r a t u r e .

Bane, R. W., Argonne National Laboratory, Argonne, I l l i n o i s

Bingham, C. D., Atomics Internat ional , Canoga Park, Cal i fornia

Bratton, W. D. , ’Allison ‘Division, GMC, Indianapolis, Indiana

Coyle, F. T., Kawecki Chemical Co., Boyertown, Pennsylvania

Dutina, D., Val leci tos Atomic Laboratory, GE, Pleasanton, C a l i f .

Fletcher, W., UKAEC, Capenhurst, Cheshire, England

Gregg, C. , United Nuclear, White Plains, New York

Hand, R. Bo , General E l e c t r i c Co., Cincinnati, Ohio

I s 1 1 , -

Hobart, E. W., P r a t t and Whitney Co., CANEL, Middletown, Conn.

Houston, C . D., A i r Force Materials Lab., Wright-Patterson AF’B, Ohio

Kelley, K. J., P r a t t and Whitney Co., CANEL, Middletown, Conn.

Kuivinen, D. E., Lewis Research Center, NASA, Cleveland, Ohio

McGee, J., United Nuclear, White Plains, New York

Murie, R. A., Allison Division, GMC, Indianapolis, Indiana

Newman, L., Brookhaven National Laboratory, Upton, Long Island, N. Y.

Stenger, V. A., Dow Chemical Company, Midland, Michigan

Tepper, F., Mine Safety Appliance Research Corp., Callery, Pa.

Thorley, A., UKAEA, Culcheth, Warrington, England

Waterbury, G. R., Los Alamos S c i e n t i f i c Laboratory, Los Alamos, N. M. I I

INTHODUCT I ON

There is at present an increasing interest in the determination of

impurities in the alkali metals in the order of 10 ppm or less. This

interest has raised the question of the influence of atmospheric

impurities, within the dry box in which the samples are handled, on

the reliability of the analytical methods for the determination of these impurities. The-impurities most likely to be present, and which would

have an influence on the analytical results, are moisture, oxygen,

hydrogen, nitrogen and carbon dioxide. We must therefore establish

maximum permissible concentration levels for these impurities in order

to increase the reliability of the analytical methods.

In order to fully explore the problem of the effects of these impurities on the analytical methods so as to establish,maximum permiss-

ible concentration levels for these impurities, several factors were

considered. We took into consideration the conditions which control the

rates of reaction between the alkali metals and the impurities as well

as the types of environmental systems that are presently in use for the

handling of the metals.

are used for the determination of these impurities and checked on the

ability to detect and reduce the.concentration of the impurities,

was done through a comprehensive study of readily available literature as well as direct contact with individuals actively engaged in working with the alkali metals.

:\re also examined the analytical techniques which

This

. .

IMPURITIES

Mo i s tur e

The presence of moisture as a contaminant in dry box atmospheres has the most serious effect of the impurities on the handling of alkali

metals. Not only will moisture react rapidly with the alkali metals at

low concentrations, but it will also enhance the reactions of' the other

impurities with the alkali metals.

reaction between the alkali metals and the other impurities under con-

sideration until well above the melting points of the metals.

There is apparently little or no

However,

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as l i t t l e as 10 t o 15 ppm of moisture w i l l cause the a l k a l i metals t o

react w i t h o ther of the impurit ies, such as oxygen and carbon dioxide,

a t room temperature. It has been suggested t h a t t h i s increased react ion

r a t e i s due i n par t t o the hydrogen which i s l i b e r a t e d when the moisture

reac ts with the alkali metal.

. . Oxygen

The f a c t o r s which influence the react ion of the a l k a l i metals with

I n the absence of moisture at room temp- oxygen are somewhat involved.

e r a t u r g highly protective, t h i n film oxide coatings w i l l form on the

a l k a l i metals. There i s l i t t l e or no react ion a f t e r t h i s i n i t i a l oxygen .

uptake. A s the melting points are approached, t h e cracking of t h i s oxide

f i l m w i l l cause f u r t h e r react ion between the dry oxygen and the exposed

metal. This react ion r a t e increases with an increase i n temperature.

The r a t e of react ion increases a l s o with t h e increase i n molecular

weight of the a l k a l i metal.

as 0.005 mm caused sodium t o react with dry oxygen a t 270 C while no re -

ac t ion w a s apparent even at 550 C i n t h e absence of t h e hydrogen. It has

a l s o been shown t h a t a few ppm of nitrogen w i l l s e n s i t i z e t h e surface of

sodium metal and cause an increased react ion with dry oxygen.

taminants may w e l l have a similar e f f e c t on t h e react ion of the a l k a l i

The presence of hydrogen a t as low a pressure 0

0

Other con-

metals with dry oxygen.

f o r up t o 10 hours, while l i thium of 99.9$ pur i ty blackened i n seconds.

Hydrogen

Lithium of 99.99% pur i ty remained br ight i n a i r

The react ion between hydrogen and the alkali metals i s negl igible a t

room temperature. I ts react ion with e i t h e r lithium, sodium or potassium

i s not d i scern ib le u n t i l t h e i r respective melting points a r e reached,

while the reac t ion with both rubidium and cesium i s suppressed u n t i l a

temperature of almost 60oOc. an ts has no e f f e c t on t h e react ion of' hydrogen with the a l k a l i metals.

The presence of any of the other contamin-

Nitrogen

When ne i ther argon nor helium a r e available, nitrogen may be used as

an i n e r t atmosphere within dry box systems when l i thium i s not involved.

Lithium w i l l r eac t with nitrogen at room temperature t o form a very thin,

protect ive coating of n i t r i d e i n the absence of moisture.

and extent of t h i s react ion w i l l increase rapidly a t elevated temperatures

o r i n the presence of e i t h e r a small amount of oxygen or as l i t t l e as

Both the r a t e

(1

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10 ppm of moisture.

oxygen i n t he presence of nitrogen.

i s no reac t ion between nitrogen and the o ther a l k a l i metals even at some-

what e levated temperatures or i n t h e presence of other of t h e contaminants.

We have reported on t h e reac t ion of sodium with

For a l l p r a c t i c a l purposes there

Carbon Dioxide

Dry carbon dioxide w i l l r eac t with l i thium, sodium and potassium at 0 temperatures i n t h e order of 300 C ana above and with rubidium and cesium

at somewhat lower temperatures. A t room temperature t h e reac t ion with

t h e a l k a l i metals i s dependent on t h e presence of moisture t o f i r s t form t h e a l k a l i metal hydroxide which w i l l i n t u r n reac t with t h e carbon

dioxide. Under c e r t a i n conditions, carbon monoxide w i l l r eac t with t h e

a l k a l i metals at elevated temperatures t o form carbonyls.

ENVIRONMENTAZ SYSTEMS

A t present, four types of environmental systems are i n common use for t h e handling of t h e a l k a l i metals. These a re : a remotely operated high-

vaxuum box; a high vacuum-inert atmosphere glove box; a vacuum-inert

atmosphere glove box i n which t h e i n e r t gas i s continuously recycled

during operation through a pur i f i ca t ion apparatus, and an i n e r t atmosphere

box equipped with both an evacuable t r a n s f e r chamber and a gas recycl ing

and pu r i f i ca t ion system. The remotely operated box i s always under vacuum

and the containment systems t o be sampled a re introduced i n t o t h e box

through an evacuable t r a n s f e r chamber. The sample i s t r ans fe r r ed from

t h e container t o a reac t ion vesse l by e i t h e r extrusion or melting.

Encapsulation of samples within the box i s accomplished by e l ec t ron beam

welding

The high vacuum-inert atmosphere box i s normally under vacuum when

not i n use. The purif ied, i n e r t gas i s admitted t o t h e box j u s t p r i o r t o

use, and manipulation within t h e box i s accomplished through rubber

gloves. An evacuable t r a n s f e r chamber i s a l s o a p a r t of t h i s box.

Welding within t h i s type of box i s done by e i t h e r helium or argon arc,

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8

depending on t h e i n e r t gas used i n conjunction with the box.

The recycl ing gas systems are becoming more and more popular. The

i n e r t gas i s continuously recycled through a commercial u n i t which I

normally removes oxygen, moisture, hydrogen and carbon dioxide t o pa r t s -

per-mill ion quan t i t i e s . Again, t h e vacuum-inert atmosphere glove box

i s under vacuum when not i n use. The pu r i f i ca t ion apparatus i s operated

\I

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only when the box contains an i n e r t atmosphere. The . iner t atmosphere

box with an evacuable t r a n s f e r chamber i s p a r t i a l l y evacuated and then

flushed with t h e i n e r t gas f o r several such cycles. The box i s then

maintained under an i n e r t atmosphere of t h e continuously recycling gas

f o r extended periods of time whether or not the box i s i n a c t u a l use.

DISCUSSION

With t h e exception of the remotely operated extrusion sampler and

t h e vacuum amalgamation technique f o r the determination of oxygen used

a t Lewis-NASA, t h e d i s t i l l a t i o n method, and c e r t a i n in- l ine i n s t r u -

mentation techniques, other a n a l y t i c a l methods f o r t h e determination of

contaminants i n the a l k a l i metals a r e a t one time or another subject

t o exposure t o an i n e r t atmosphere. The more rout ine methods involve

. t h e determination of oxygen, carbon and hydrogen. I n each case t h e

sample f i rs t must be t ransfer red t o a su i tab le react ion apparatus.

The analysis i s usual ly car r ied out under an i n e r t atmosphere ei thek

within o r outside of t h e dry box i n which t h e sample was t ransfer red t o

t h e react ion vessel. Both helium and argon are acceptable cover gases

with heliqun being preferable i n systems vhich incorporate l i q u i d nitrogen

cold t raps .

Fortunately, modern instrumentation and technology affords us t h e

a b i l i t y t o de tec t and remove microgram amounts of the contaminants j u s t

discussed from t h e high p u r i t y systems under consideration. There a r e

many commercially avai lable t r a c e oxygen analyzers, hygrometers and gas

chromatographs. These instruments a r e capable of detect ing as l i t t l e as

1 ppm of these contaminants. Several commercial gas pur i f ica t ion and

recycling apparat i are a l s o avai lable which are capable of reducing t h e

concentration of these contaminants t o l e s s than 1 ppm.

can r e s o r t t o hot titanium, uranium or zirconium g e t t e r t raps , as w e l l

as molecular sieve and cold t raps , t o reduce t h e concentration of the

contaminants i n t h e i n e r t gas p r i o r t o t h e introduction of t h i s gas i n t o

the high pur i ty system.

I n addition, we

The problems a r e d i f f e r e n t f o r the high-vacuum, remotely; operated

$-r[ Doxes and the vacuum a n a l y t i c a l systems. It has been found t h a t a

vacuum of at least 1 x t o r r i s necessary f o r reproducible a n a l y t i c a l

r e s u l t s . However, it i s possible t o use a vacuum system which i s capable

of only lom3 t o r r i f t h e system i s flushed several times with an i n e r t

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gas of high pur i ty . Conversely, a system capable of operating a t lo-'

t o r r which i s pumping a t lom5 t o r r subjec ts t h e sample t o a continuous

leak and contamination while t h e o r e t i c a l l y operating a t a pressure void

of contamination. Fortunately, l eak- t igh t , high vacuum systems a re no

longer d i f f i c u l t t o obtain a t r e l a t i v e l y low cos ts .

FUEOMMENDATIONS AND CONCLUSIONS

The following values, recommended f o r t h e m a x i m u m concentration

l e v e l s of t h e impurit ies, a r e based on normal dry box operations and

minimum exposure time of t h e a l k a l i metal sample during t r a n s f e r of t h e

sample t o the reac t ion system: moisture, l e s s than 5 ppm; oxygen, l e s s

than 10 ppm; hydrogen, less than 5 ppm; nitrogen, less than 10 ppm ( i n

t h e handling of l i th ium); and carbon dioxide, l e s s than 10 ppm.

Exceptions can be made. I f , f o r example, one w e r e analyzing f o r carbon,

l a r g e r concentrations of oxygen, hydrogen o r even moisture could be

t o l e r a t e d , i n the absence of carbon dioxide. One should a l s o r e a l i z e

t h a t a sample t r ans fe r r ed i n t o a s m a l l r eac t ion vesse l f o r subsequent

ana lys i s f o r oxygen by t h e amalgamation procedure i s exposed t o far l e s s

of t h e contaminant than a sample which i s amalgamated within t h e dry box.

Also, sol id , cold samples are less l i k e l y t o r eac t with t h e contaminants.

than molten samples.

Although w e have mentioned various techniques by which t h e concen-

t r a t i o n s of these contaminants can e a s i l y be reduced t o wel l below the

des i red leve ls , t he re are problems at tendant t o maintaining these low

l e v e l s . W e have already discussed the p o s s i b i l i t y of contamination i n

t h e high-vacuum systems. Returning t o t h e high-purity i n e r t gas systems,

we f i n d t h a t aside from leaks i n t h e box or t h e vacuum system, which can

be r ead i ly corrected, t he main source of contamination i s t h e rubber

gloves used t o manipulate t h e sample wi th in t h e box. Tests with neoprene

and bu ty l rubber gloves show t h a t while t h e increase of oxygen, hydrogen,

ni t rogen and carbon dioxide through d i f fus ion i s negl igible , t h e d i f fus ion

of moisture i s a matter f o r concern.

The bu ty l rubber gloves appear t o be preferable t o t h e o ther types

of ava i lab le gloves. However, these same gloves have been found t o add

0.01 g. of w a t e r vapor per hour t o a dry box when exposed t o average

temperature and humidity.

are i n use.

This value increases tenfo ld when t h e gloves

The permeation rate i s dependent on both t h e p a r t i a l :

-9-

pressure d i f f e r e n t i a l of the water vapor across t h e glove and the

thickness of the glove. Neoprene gloves have been known t o add moisture

a t the r a t e of 50 ppm per hour.

have t h e addi t ional disadvantage of ‘ react ing with the more ac t ive a l k a l i

metals, espec ia l ly cesium. A t present t h e only known solut ion t o the

glove problem i s t h e use of a second p a i r of gloves within the glove

attached t o the dry box. Of f u r t h e r value i s t h e f l o w of a continuous

stream of dry a i r or i n e r t gas between t h e two p a i r s of gloves.

Gloves made of polymers with halogens

A t first glance it would appear t h a t f o r general use t h e dry box

which incorporates t h e recycling p u r i f i c a t i o n system i s the panacea for

a l l our problems.

t h i s might wel l be t h e case. While it i s t r u e t h a t the pur i f ica t ion

uni t w i l l remove t h e moisture as wel l as the other contaminants from

t h e dry box atmosphere t o wel l below t h e suggested m a x i m u m levels , we

must remember t h a t addi t iona l w a t e r vapor i s continuously d i f fus ing

through the gloves i n t o t h e box, and, of necessity, i n close proximity

t o t h e samples being handled through t h e use of t h e gloves. However,

t h i s type of dry box can be used f o r an hour or more before one notes

With the exception of water vapor contamination,

discolorat ion of t h e a l k a l i metal due t o contamination.

of box need not be evacuated between samplings, the glove ports should

be sealed and kept under vacuum when t h e box i s not i n use. This type

of sample handling system does, however, have a d e f i n i t e advantage over

t h e regular vacuum-dry box which can be used for only a short period of

t i m e before d isco lora t ion i s noted and which must be evacuated between

samplings. .The use of a second p a i r of gloves almost doubles the working

t i m e i n both these systems before contamination i s noted.

While t h i s type

I n making these recommendations it i s by no nieans f e l t t h a t our

problems a r e solved. The continuous development of more precise methods

may eventually warrant a need f o r even lower l e v e l s of contamination.

A t t h i s time it would be impractical t o suggest t h a t we es tab l i sh l e v e l s

of l e s s than 5 ppm when such a high degree of p u r i t y does not seem t o be

necessary. Nor i s it recommended t h a t everyone be made t o incorporate

a gas recycling p u r i f i c a t i o n u n i t i n t o t h e i r dry box operation. We do

believe t h a t a l l alkali metals work should be r e s t r i c t e d t o high vacuum-

high pur i ty systems such as j u s t discussed. It i s f u r t h e r recommended

t h a t two p a i r s of gloves should be used during sample handling and t h a t

addi t ional work should be done toward t h e development of a b e t t e r dry

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box glove.

between t w o l ayers of rubber?)

t o standardize t h e methods of sampling and ana lys i s with consideration

given t o t h e equipment and funds t h a t may be ava i lab le t o t h e average

a n a l y t i c a l f a c i l i t y .

(What of a laminated glove with a moisture b a r r i e r sealed

And f i n a l l y , it would be b e n e f i c i a l

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APPENDIX

Bibliography

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Alkali Metal-Gas Reactions, Par t X: Reaction of Sodium with Oxygen, P. B. Longton, UKAEPI, IGR-TN/C-536.

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Notes on Liquid Metal Studies i n France and Great Britain, L. F. Epstein, NASA, Tech. Memorandum X-884 (June, 1963).

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0 0

0 Oxidation Rate of Sodium Between -79 C and MoC, J. V. Cathcart, L. Lo Hall, G. P. Smi.th, Acta Meta. - 59 245 (1957).

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Reaction of Potassium with Wet Oxygen, P. B. Longton, UKAEA, IGR-TM/C-- 039 0

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Techniques of Inorganic Chemistry, Vol. I11 (Chapter on Glove Box Techniques), Jonassen and Weessberger, Interscience (1963).

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Titrimetric Determination of Traces of Nitride Nitrogen in Sodium Metal, C. H. Ward, R. D. Gardner, W. H. Ashley, A. Zerwekh, LASL, LA-2892.

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EXTERNAL DISTRIBUTION (CONTINUED)

H. Kirtchik, G. E., Cincinnati, Ohio D. E. Kuivinen, NASA, Lewis, Cleveland, Ohio J. F. Lagedrost, BMI, Columbus, Ohio R. C. Lindberg, NASA, Lewis, Cleveland, Dhdo J. McGee, United Nuclear, White Plains, N. Y. J. McSorley, Westinghouse, APD, Pit tsburgh, Pa. S. A. Meacham, APDA, Trenton, Michigan B. Minushkin , United Nuclear, White Plains, N. Y. J. H. Monaweck, ANL, Argonne, I l l i n o i s R. A. M u r i e , Allison Div., GMC, Indianapolis, Indiana L. Newman, BNL, Upton, L. I., N. Y. C. Palladino, MSA Research Corp., Callery, Pa. T: FdSP~rach; BNL, Upton, I;. I . ,N . Y. S. Rodgers, MSA Research Corp., Callery, Pa. L. Rosenblum, NASA, Lewis , Cleveland, Ohio V. J. Rutkauskas, LASL, Los Alamos, New Mexico J. M. Scarborough, Atomics Internat ional , Canoga Park, C a l i f . E. M. Simons, BMI, Columbus, Ohio E. L. Steele , General Atomics, San Diego, C a l i f . V. A. Stenger, Dow Chemical Co., Midland, Michigan F. Tepper, MSA Research Corp., Callery, Pa. A. Thorley, UKAEA, Culcheth, Warrington, England G. R. Waterbury, LASL, Los Alamos, New Mexico G. Zel lars , NASA, Lewis, Cleveland, Ohio

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