The Development of a Purification Method of Lithium EUR 4072

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PURIFICATION

METHOD OF LITHIUM

PAUWELS and K. F. LAUER

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Central Bureau for Nuclear Measurements - CBNM

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EUR 4072 e

THE DEVELOPMENT OP A PURIFICATION METHOD OF

LITHIUM by J. PAUWELS and K.F. LAUER

European Atomic Energy Community — EURATOM

Joint Nuclear Research Center — Geel Establishment (Belgium) Central Bureau for Nuclear Measurements — CBNM

Brussels, September 1968 — 22 Pages — 3 Figures — FB 40

A purification method of lithium on a cation-exchange resin in 1 M HCl was described. To allow the preparation of lithium containing

Z. 50 ppm alkali and alkali-earth metals, a special purification of the ion-exchanger was needed. A method using batch operations with the tetra lithium salt of EDTA, with 30 % hydrochloric acid, and elution with 1 M hydrochloric acid was described.

EUR 4072 e

THE DEVELOPMENT OF A PURIFICATION METHOD OF LITHIUM by J. PAUWELS and K . F . LAUER

A purification method of lithium on a cation-exchange resin in 1 M HCl was described. To allow the preparation of lithium containing ^ 50 ppm alkali and alkali-earth metals, a special purification of the ion-exchanger was needed. A method using batch operations with the tetra lithium salt of EDTA, with 30 % hydrochloric acid, and elution with 1 M hydrochloric acid was described.

EUR 4072 e

THE DEVELOPMENT OF A PURIFICATION METHOD OF LITHIUM by J. PAUWELS and K . F . LAUER

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EUROPEAN ATOMIC ENERGY COMMUNITY - EURATOM

THE DEVELOPMENT OF A PURIFICATION

METHOD OF LITHIUM

by

J. PAUWELS and K. F. LAUER

1968

Joint Nuclear Research Center Geel Establishment - Belgium

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SUMMARY

¿1 50 ppm alkali and alkali-earth metals, a special purification of the ion-exchanger was needed. A method using batch operations with the tetra lithium salt of EDTA, with 30 % hydrochloric acid, and elution with 1 M hydrochloric acid was described.

KEYWORDS

REFINING IMPURITIES

SEPARATION PROCESSES LITHIUM

ION EXCHANGE MATERIALS EDTA

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C o n t e n t s

page

1. Introduction 1

2. P r i n c i p l e of the method 2

3. E x p e r i m e n t a l details of the method 2 3. 1. E l e m e n t s of i n t e r e s t and their determination 2

3 . 2 . Determination of distribution coefficiente 2 3 . 3 . Determination of purification factors (PF) 4

3.4. Purification of AG 50W-XI6 5

4. R e s u l t s and conclusion 7

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5

-1. I n t r o d u c t i o n

In a previous r e p o r t , four methods of determination of 0. 1 M lithium hydroxide solutions with a final a c c u r a c y of 0.02% w e r e d e s c r i b e d . As these methods, which a r e not s e l e c

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tive, have to be applied to Li and Li solutions for the p r e paration of isotopie blends, and no chemically pure Li or 7

Li s a m p l e s were available, a purification method of lithium was needed.

The purity of the final lithium has to be such, that the r e s i dual i m p u r i t i e s do not cause any hygroscopy that might d i s t u r b g r a v i m e t r y of the formed lithium s a l t s , and that c o r r e c t i o n s for systematic e r r o r s a r e practically negligible. F u r t h e r , the lithium has to be in such a form that its t r a n s formation into a pure 0. 1 M aqueous hydroxide solution i s p o s s i b l e .

L η

The m o s t important i m p u r i t i e s found in enriched Li or Li s a m p l e s were a l k a l i - and a l k a l i - e a r t h m e t a l s (up to 0. 15% together).

Different s e p a r a t i o n s of lithium from these elements were r e p o r t e d e a r l i e r , but they were m o s t l y limited to one or two e l e m e n t s , and few authors give indications about the absolute purity of the separated lithium fraction. Most of

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these methods a r e based on extraction , precipitation (7-12) , . . . (13-35)

x , or ion exchange chromatography

N e v e r t h e l e s s , the most recent of them all concern s e p a r a tions on cation exchange r e s i n s in the hydrogen form. An i m p o r t a n t study of the behaviour of the alkali m e t a l s in p r e s e n c e of Dowex 50 and Duolite C3 in the system HCl·

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H90 - CH OH was done by Nelson v '. The described s

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2. P r i n c i p l e of t h e M e t h o d

In diluted hydrochloric acid the alkali m e t a l s a r e r a t h e r strongly absorbed by cation-exchanger s like Dowex 50,

whereby lithium i s the l e a s t a b s o r b e d one. F r o m the values (35) of the distribution coefficients as d e t e r m i n e d by Nelson for Dowex-X4 it can be seen that quantitative s e p a r a t i o n s m u s t be p o s s i b l e .

To obtain still higher selectivities it i s useful to use a r e s i n with a higher DVB-content ("X16").

The described purification was p e r f o r m e d on AG 50W-X16 (50/100 m e s h ) , a Dowex 50W-X16 specially purified for a n a lytical p u r p o s e s . N e v e r t h e l e s s , further purification of this r e s i n was n e c e s s a r y .

This was made by batch operations w i t h E . D . T . A . in Li OH medium, concentrated hydrochloric acid and final elution with

1 M hydrochloric acid.

3. E x p e r i m e n t a l D e t a i l s of t h e M e t h o d

3 . 1 . E l e m e n t s of i n t e r e s t and their determination

3 . 1 . 1 . Lithium

Lithium was localized in the eluate and d e t e r m i n e d for the calculation of the distribution coefficients by t r a n s f o r m a t i o n into and calcination as sulfate.

In the case of the Κ , - d e t e r m i n a t i o n s 5 m l fractions containing 7 to 15 mg of lithium sulfate were analysed. Under these con ditions a p r e c i s i o n of 1-2% can be obtained.

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45

with a Nal(Tl) Well-type scintillation counter, Ca by r e l a tive β -counting. During the separation test Li/Mg, m a g n e s i u m was determined photometrically with titan yellow.

3 . 1 . 3 . T r a c e analysis in i o n - e x c h a n g e r s and purified lithiums Ion-exchangers were calcined and purified lithiums dried as lithium chloride. The r e s i d u e s were analysed for m e t a l lic i m p u r i t i e s by the e m i s s i o n spectrographic service of the C . B . N . M .

3 . 2 . Determination of distribution coefficients (Κ ,)

Distribution coefficients for lithium, sodium, potassium, b e r y l l i u m , m a g n e s i u m and calcium were determined for c o m m e r c i a l grade D o w e x 5 0 W - X l 6 by batch equilibration t e s t s on

1-2 g r a m s oven dried r e s i n and 10 m l of hydrochloric acid. Κ ..-values were calculated from relative m e a s u r e m e n t s of _α identical fractions of blanks and samples using the formula:

M -M m l Κ

d M1 g

in which:

M. = the total amount of the ion _t

M, = the amount p r e s e n t in the liquid

m l = the number of m i l l i l i t e r s of hydrochloric acid. g= the number of g r a m s of oven-dried r e s i n .

A s u m m a r y of the obtained r e s u l t s is given in figure 1. Separation factors β = Κ , /Κ a r e s u m m a r i z e d in figure 2.

M Li

F r o m this figure it can be seen that an efficient separation

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large K , - v a l u e for lithium leads to broadening of the lithium peak in the effluent. 1 M hydrochloric acid was chosen as eluant. The K , - and ß-values derived from figures 1 and 2 for this medium were s u m m a r i z e d in Table I.

3. 3. Determination of purification factors (P. F . )

3 . 3 . 1 . Method of separation

Separations were p e r f o r m e d on 3 cm d i a m e t e r quartz columns filled with a quantity of r e s i n equivalent to 80 g r a m s of oven-dried Dowex 50W-X16 ( « 4 0 0 m e q . ) . Before the separation begins the r e s i n is washed with bidistilled water, until chloride ions a r e fully r e m o v e d .

On the other hand 0.5 g of lithium and 100 to 500 /Ug of a t r a c e d a l k a l i - or alkali e a r t h m e t a l a r e a b s o r b e d on 16 g r a m

oven-dried Dowex 50W-X16 ( « 8 0 m e q . ) by mixing during 30 m i n u t e s . After settling of the r e s i n and décantation of the solution, the wet r e s i n is t r a n s f e r r e d to the top of the column. The elution i s performed with (1.00 + 0.02) M hydrochloric acid.

The effluent i s collected in 50 m l polyethylene r e c i p i e n t s .

3 . 3 . 2 . Determination of purification factors

Separations of L i / Na, L i / K, L i / Be, Li/Mg and L i / Ca m i x t u r e s were made under the conditions described above. Generally 85-90% of the lithium were localized in the fractions 69 or 710, and the concentration was at a m a x i m u m in f r a c -tion 8 or 9.

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3 . 4 . Purification of AG 50W-X16

3 . 4 . 1. Introduction

A first t e s t separation using AG 50W-X16 (50/100 m e s h ) , twice washed with isopiëstically distilled 4 N HCl, was done under the conditions described in 3 . 3 . 1 . Isopiëstically distilled 1 N HCl was used as eluant. The r e s u l t s a r e s u m m a r i z e d in Table III.

The high calcium content of the s o - c a l l e d purified product could be explained by e m m i s s i o n s p e c t r o g r a p h s analysis of the AG 50W-X16, which contained up to 1 eq. % of calcium. The r e s i d u a l i m p u r i t y level in the purified lithium is due to

two s o u r c e s (fig. 3): MT depending on the purification factor

( P . F . ) and M_ proportional to the i m p u r i t y content of the ion exchanger and i n v e r s e l y proportional to the distribution coef-ficient (K,) of this impurity. In our case - high P . F . and i m p u r i t y content of impurified lithium in the 0.1 % range -the first factor is negligible, and only -the r e s i n purity has an influence on the purity of the purified lithium. F o r this r e a s o n it was i m p o r t a n t to improve the purity of the ion-exchanger used.

Two methods were tested for this purpose:

- batch operations with hydrochloric acid of appropriated concentration

- batch operations w i t h E . D . T . A . at appropriated pH.

3 . 4 . 2 . Hydrochloric acid method

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-used.

It was decided t o proceed with a 5 : 1 r a t i o 5 M HCl a i r dried AG 50W-X16.

T e s t purifications were c a r r i e d out with ' s u p r a p u r ' HCl (Merck A. G . / G e r m a n y ) and with i s o p i ë s t i c a l l y distilled HCl. 10 g r a m fractions of r e s i n were mixed for two h o u r s by m a g -netic s t i r r i n g with 50 m l HCl in closed teflon containers and decanted after settling. After each batch operation the r e s i n was r i n s e d with 50 m l bidistilled w a t e r . After the l a s t batch operation this rinsing was repeated t h r e e t i m e s .

The r e s i n was then t r a n s f e r r e d to a platinum crucible, dried for one night at 100°C and calcined. I m p u r i t i e s were d e t e r -mined by e m i s s i o n spectrography. The r e s u l t s s u m m a r i z e d in Table IV show that the calcium contamination i s lowered by a factor 20-40. No i m p o r t a n t lowering of the impurity content of the other alkali m e t a l s i s obtained.

3 . 4 . 3 . E . D . T . A . method

Ethylene diamine t e t r a acetic acid being sparingly soluble in water, and the stability of its calcium complex i n c r e a s i n g with i n c r e a s i n g pH, it seemed n e c e s s a r y to neutralize EDTA with a b a s e .

NH OH has the inconvenience that eventually contaminating NH . ions cannot d i r e c t l y be d e t e r m i n e d by e m i s s i o n s p e c t r o -graphy or activation a n a l y s i s .

Finally LiOH was p r e f e r r e d : it can easily be d e t e r m i n e d by e m i s s i o n spectrography, and the Li -ion is the e a s i e s t one to rinse from the ion exchange r e s i n with hydrochloric acid.

3 . 4 . 3 . 1 . Influence of the pH

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of LiOH i n 50 m l of w a t e r . A s the d i s t r i b u t i o n coefficient

of l i t h i u m for AG 50WX16 i s v e r y high in n e u t r a l and

a l k a l i n e m e d i u m , one can c o n s i d e r that 30 m m o l of LiOH

n e u t r a l i z e s the r e s i n , and the r e s t f o r m s r e s p . H „Y, 4

LiH Y, L i2H Y, LÌ3HY and L i4Y .

After settling of the r e s i n and décantation of the solution,

the r e s i n was r i n s e d with b i d i s t i l l e d w a t e r to e l i m i n a t e

E . D . T . A . Two o t h e r batch o p e r a t i o n s with 30% HCl ' s u p r a

p u r ' w e r e m a d e to e l i m i n a t e Li, Na, K and Mg, which have

v e r y low d i s t r i b u t i o n coefficients in t h i s m e d i u m . The Κ ,

value of Ca being high, one can e a s i l y a p p r e c i a t e the i n

fluence of the E . D . T . A . t r e a t m e n t on the e l i m i n a t i o n of

c a l c i u m f r o m the r e s i n (Table V).

3 . 4 . 3 . 2 . R e s u l t s for L i . Y

Two batch o p e r a t i o n s with Li Y, followed by two o t h e r s with

3 0 % h y d r o c h l o r i c a c i d (Merck A G S u p r a p u r ) allow r a t h e r

good p u r i f i c a t i o n s of AG 50WX16.

N e v e r t h e l e s s , it was n e c e s s a r y to p e r f o r m a s u p p l e m e n t a r y

r i n s i n g of the p u r i f i e d i o n e x c h a n g e r with 1 M ' s u p r a p u r '

HCl to e l i m i n a t e c o m p l e t e l y the lithium i o n s . This s u p p l e

m e n t a r y elution leaded to a gain of a f a c t o r 10 on the sodium

e l i m i n a t i o n too.

A c o m p a r i s o n of the i m p u r i t y l e v e l s of the o r i g i n a l r e s i n

v e r s u s the purified r e s i n i s given in Table VI.

4. R e s u l t s a n d C o n c l u s i o n

400 g r a m aliquote of AG 50WX16 cation e x c h a n g e r w e r e p u r i ·

fied by s u c c e s s i v e batch o p e r a t i o n s with:

1. 400 m m o l E . D. T. A. and 2800 m m o l LiOH i n a t o t a l

volume of 2 1.

2. 400 m m o l E . D . T . A . and I6OO m m o l LiOH i n a total

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3. 2 1 30% 'Suprapur' hydrochloric acid. 4. 2 1 30% 'Suprapur' hydrochloric acid.

After the first t h r e e batch operations the i o n - e x c h a n g e r was washed with 1 1 bidistilled water, and after the third one t h r e e t i m e s . Then, quartz columns were filled with quanti-ties equivalent to 80 g r a m s of the o v e n - d r i e d r e s i n ,

(«400 m e q . ) and e lut e d with 3 1 1 M. hydrochloric acid and 0.5 1 bidistilled w a t e r . The whole operation was m a d e in a glove box to avoid contamination from the a t m o s p h e r e . On the other hand, quantities of 25 g a i r - d r i e d unpurified AG 50W-X16 ( « 8 0 m e q . ) were mixed for 30 minutes with approximately 75 m m o l LiOH solution in 20-25 m l .

After settling of the l i t h i u m - c h a r g e d r e s i n , the supernatant solutions were decanted, and the wet r e s i n s t r a n s f e r r e d to the top of the different columns.

Elutions were p e r f o r m e d with (1.00 + 0.02) M HCl ' s u p r a -p u r ' , and eluates collected in -polyethylene reci-pients of 50 m l . 1 m l aliquote were analysed by t r a n s f o r m a t i o n to and weighing as lithium sulfate.

Generally, 80 - 90% of the starting lithium were r e c o v e r e d in fractions 7-9 or 8-10 of the eluate, with m a x i m u m

con-centration in fractions 8 or 9. 7 6

2 g Li and 1.8 g Li were purified following this scheme, and analysed by e m i s s i o n s p e c t r o g r a p h y (Table VII).

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a l k a l i and a l k a l i e a r t h m e t a l s , which can be u s e d for the

p r e p a r a t i o n of s p e c t r o g r a p h i c s t a n d a r d s . The s i l i c i u m

found i s p r o b a b l y due to the u t i l i z a t i o n of q u a r t z c o l u m n s .

The u s e of teflon columns will p r o b a b l y e l i m i n a t e t h i s , but

the quantity found i s u n i m p o r t a n t for v o l u m e t r i c a s well a s

for g r a v i m e t r i c a n a l y s e s with p r e c i s i o n s of 0.02 %

A c k n o w l e d g e m e n t s

The a u t h o r s a r e indebted to J . Spaepen for initiating t h i s

w o r k . T h e y thank Prof. J . H o s t e , G . H . Debus, P . J . De B i è v r e

and Y. Le Duigou for c r i t i c a l d i s c u s s i o n s .

T h e y a l s o thank Ch. B e r t h e l o t , S. H e r m a n n and T. M e n c a r e l l i

for e m i s s i o n s p e c t r o g r a p h i c a n a l y s e s .

R e f e r e n c e s

(1) P a u w e l s , J . Α . , Le Duigou, Y. and L a u e r K . F .

E U R 3 6 5 6 e (1967).

(2) P l u i s h e v and Shakhno

Z h u r . A n a l . K h i m . n° 8, 5 (1953)

(3) C a l e y E . R . and Axibrod H . D .

Ind. eng. C h e m . , a n a l . E d i t . J_6, 712 (1944)

(4) H a g i w a r a Z . and Kato T.

Bunseki to Shirjakn 2, 179 (1948)

(5) Kato T . and H a g i w a r a Ζ.

T e c h n o l . R e p t s . Tohoku Univ. 1_4 (2), 14 (1950)

(6) Guther G . A . and H a m m o n d G . S .

J . A. C . S . 78, 5166 (1956)

(7) P e c h i n a y (Compagnie de p r o d u i t s c h i m i q u e s et é l e c t r o

m é t a l l u r g i q u e s ) F r . 1 137 089 (1957)

(8) B o n n i e r E .

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14

(9) Sandell E . B .

C o l o r i m e t r i e d e t e r m i n a t i o n of t r a c e m e t a l e 3 0 1 , NY (1944)

[10) C i m e r m a n C. and Wenger P .

M i k r o c h 24, 162 (1938)

[11) W i l a r d H . H . and Goodspeed E . W .

Ind. eng. C h e m . , a n a l . E d i t . 8, 414 (1936)

[12) O s t r o u m o v Ε . Α .

Ann. C h i m . A n a l . 20 (3) 9 (1953)

[13) S a m u e l s o n O. and S j ö s t r ö m E .

A n a l . C h e m . 26, 1908 (1954)

[Ϊ4) Samuelson O. and S c h r a m m K. Ζ. E l e c t r o c h e m . J57, 207 (1953)

[15) Nelson F .

J . A . C S . 77, 813 (1955)

[16) Kawabe Η . , Gualandi C. and Buna Ann. Chim. (Roma) 53_, 368 (1963)

Bosholm J.

J. C h r o m a t o g r . 21 (2), 286 (1966)

(18) Etienne Η.

Ind. Chim. Belge, Suppl. n° 1, 165 (1959)

(19) Dietrich W . C . and B a r r i n g e r R . E . Y-1254 (1959)

(20) Gorshkov V . l . , Kuznetsov, I . A . , Panchenkov G. M. and Kustova I . V .

Zh. Neórg. Khim. 8 (12), 2790 (1963)

(21) Bagbanby I. L . , Guseinov I.K. and Posadovskaya A , K . A z e r b . Khim. Zh. n° 6, 93 (1963)

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(23) T o l m a c h e v A . M .

V e s t n . Mosk. U n i v . , S e r . II, Khim 19_ (2), 20 (1964)

(24) H e r i n g H.

A n a l . c h i m . Acta 6, 340 (1952)

(25) Maslova G . B . , Suslova Ε . Α . , and Chmutov K . V .

Z h u r . A n a l . K h i m . 1_2, 359 (1957)

(26) J e n t z s c h D. and F r o t s c h e v I.

Z . a n a l . C h e m . 144, 1 (1955)

(27) M a z z a L . , Sardo L . , F r a c h e R. and Dadone A.

G a z z . C h i m . I t a l . 95 (6), 599 (1965)

(28) V e n t u r e l l o G. , Gualandi C , and M a z z e i I.

Ann. C h i m . (Roma) 49, 149 (1959)

(29) B u r a n a , Gualandi C. , and M a z z e i I.

Ann. C h i m . (Roma) 53, 368 (1963)

(30) Okuno H. , Honda M. and I s h i m o r i T .

J a p a n A n a l y s t . 2, 428 (1953)

(31) R a t n e r R. and L u d m e r Z .

I s r a ë l J . C h e m . 2, 21 (1964)

(32) Sulcek Z . , R o s s and T h o m a

ORNL3656 (1965)

(33) N e v o r a l V.

Z . a n a l . C h e m . 195, 332 (1963)

(34) G o r s h k o v V . l . , Kuznetsov I . A . and Panchenkov G. M.

Z h . A n a l . K h i m . 14, 417 (1959)

(35) N e l s o n F . , M i c h e l s o n D. C , P h i l l i p s H. O. , and K r a u s K. A.

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T A B L E I

K , and p v a l u e s for Dowex 50WX16 in 1 M HCl

E l e m e n t

L i N a K B e Mg C a

Di s t r i b , coëff. K , α

2 . 4 5

6 . 4

2 2 . 3

9.6

14.0

2 3 0

S e p . factor pM / L i

1 2 . 6 9 . 1 3 . 6 5 . 7 9 4

T A B L E II

P u r i f i c a t i o n f a c t o r s for L i / N a , K, B e , Mg, Ca

for the working conditions

S e p a r a t i o n

L i /2 2N a

L i /4 2K

L i /7B e

L i / M g

L i /4 5C a

% of L i t h i u m in the 4 maxin

86 %

89 %

90 %

85 %

% of t r a c e r i u m f r a c t i o n s

0 . 3 %

< 0 . 9 %

0 . 0 0 3 %

< 1. 1 %

< 0 . 0 4 %

P . F .

2 8 0

> 100

30.000

> 80

[image:20.595.111.522.49.658.2]

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17

T A B L E IH

R e s u l t s of a t e s t s e p a r a t i o n u s i n g AG 5 0 W - X 1 6 , t w i c e w a s h e d

with i s o p i ë s t i c a l l y d i s t i l l e d 4 N HCl

E l e m e n t

N a K Mg Ca

p p m b e f o r e s e p a r a t i o n

260 90 720 120

E x p e c t e d ( b a s e d on P F )

< 1 < 1

< 1 0

< 1

p p m dtd by E m . S p e c t r o g r . a f t e r

s e p a r a t i o n

< 60

60 2400

T A B L E IV

E l i m i n a t i o n of Ca f r o m A G 5 0 W X 1 6 b y b a t c h o p e r a t i o n s w i t h 5 M H C l

ι

N u m b e r of b a t c h o p e r a t i o n s

0 1 2 3 4 5 6

p p m H C l

i n r e l a t i o n ' s u p r a p u r ' ilOOO 512 192 168 76 52 30

t o o v e n d r i e d r e s i n H C l ' i s o p . d i s t . '

« 1000 880 400 188 90 17 T A B L E V

I n f l u e n c e of t h e n e u t r a l i z a t i o n of E . D . T . A . on t h e e l i m i n a t i o n of c a l c i u m f r o m A G 5 0 W X 1 6

N e u t r . of E . D . T . A . H4Y

L i H3Y

L i2H2Y

L i3H Y L i4Y

mg C a / g o v e n d r i e d r e s i n 212

[image:21.595.71.487.132.739.2]

(22)

[image:22.595.66.521.43.707.2]

- 18

TABLE VI

Comparison of the impurity levels of the original resin versus the purified resin

Element Na K Rb Cs Mg Ca Ba Sr Si F e Al Cu

1

Original resin Purified resin (/Ug/gram of oven dried resin)

10 8 < 8 < 8 4 « 1 0 0 0 4 4 1 < 4 4 , 4 < 0.05 < 0 . 1 « 0.25 « 1 ~ 0.5

0. 1 5 - 0 . 3 < 0. 15 < 0. 1

2 . 5 0 . 3

f« 1

« 0 . 5

TABLE VII 6 7

P u r i t y of Li and Li purified by the d e s c r i b e d method

E l e m e n t

Na K Mg Ca Si F e other metals

(23)

103 102 10 1

Kd

-\ ^ _

Li

MH C l

1 103 102 10 1

«d

Be

M

_HCl

10

₁₀

IO3 102 10 I

Kd

-v_

Να

I MH C l 10 IO3 102 10 1 0

Kd

\

\ t

1 5

Mg

MH C l

10 103 102 10 !

Kd

K

ι MHCI

103 IO2 10 1

Kd

- V

V.

Ca

_ _ _ _ _ _ _ _

MH C l

1 J

10 10

(24)

200 100 80

60

40

20 10 8 6

1 0.8 0.6 Q4l·

02

0.1 Ρ M/Li

o o

MHCI

0 1 2 3 A 5

(25)

υ

c

o

TMI

ml effluent

(26)

(27)

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