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Oxygen, (hone

P.W. SCHENK

Oxyge n o2

Since oxygen c o m m e r c i a l l y a v a i l a b l e in s t e e l c y l i n d e r s c a n b e u s e d for m o s t l a b o r a t o r y p u r p o s e s a f t e r a s u i t a b l e p u r i f i c a t i o n by w a s h i n g w i t h K M n 04, KO Η and c o n c e n t r a t e d HaS 04, only two l a b o r a t o r y p r o c e d u r e s w h i c h y i e l d a p a r t i c u l a r l y p u r e g a s a r e d e s c r i b e d . T h e s e a r e an e l e c t r o l y t i c p r o c e d u r e and p r e p a r a t i o n f r o m h y d r o g e n p e r o x i d e .

I. ELECTROLYTIC OXYGEN

Of t h e n u m e r o u s d e v i c e s f o r t h e e l e c t r o l y t i c p r e p a r a t i o n of 02, t h e s y s t e m u s i n g p u r e n i c k e l e l e c t r o d e s in a 30% KOH s o l u t i o n h a s p r o v e n t o b e p a r t i c u l a r l y effective. F i g u r e 150 s h o w s t h e a p p a r a t u s . It c o n s i s t s of a g l a s s c y l i n d e r A9 about 50 c m . high and 12 c m . in d i a m e t e r , w h i c h i s 2 / 3 filled w i t h 30% KOH. T h e c a t h o d e F% i s a c y l i n d e r of Ni s h e e t s u s p e n d e d f r o m t h r e e Ni w i r e s ( o r it m a y c o n s i s t of a h e l i x m a d e of 2 - m m . - t h i c k n i c k e l w i r e ) . T h e s e t h r e e w i r e s , in t u r n , a r e a t t a c h e d t o a lid Ό m a d e of P l e x i g l a s o r p a r a f f i n - t r e a t e d h a r d w o o d . W h e n P l e x i g l a s i s u s e d , a c o n i c a l h o l e m a y b e d r i l l e d and t h e w i r e f a s t e n e d t o t h e lid by m e a n s of a m a t c h i n g g r o u n d g l a s s s t o p p e r . T h e a n o d e Fx i s p l a c e d in a g l a s s b e l l C, w h i c h i s a t t a c h e d to t h e b o t t o m of t u b e Β ( d i a m e t e r about 20 m m . ) . T h i s t u b e i s i n s e r t e d t h r o u g h t h e lid, w h i c h i s divided in two f o r t h i s p u r p o s e . T h e h a l v e s a r e t h e n r e c o n n e c t e d with two s h e e t m e t a l d i s k s . The t u b e m a y b e c e m e n t e d to t h e lid with s o m e p i c e i n . T h e a n o d e itself ( h e l i c a l o r sheet) i s s u s p e n d e d f r o m a Ni w i r e , w h i c h i s c e m e n t e d on t o p in a c o n s t r i c t i o n E. A d r o p of w h i t e s e a l i n g w a x i s p l a c e d on t h e Ni w i r e and i s p u s h e d into t h e p r e ­ h e a t e d c o n s t r i c t i o n t o f o r m a s e a l . A c o r k w a s h e r i s p u s h e d f r o m a b o v e a g a i n s t t h e s e a l i n g w a x a n d t h e w h o l e a s s e m b l y i s c o m p l e t e l y s e a l e d with p i c e i n . Some g l a s s wool i s p l a c e d in t h e bulb of t h e s i d e a r m of t u b e Β to c a t c h t h e a l k a l i s p r a y . T h e b u l b i s c o n n e c t e d to a t u b e filled w i t h p a l l a d i u m a s b e s t o s ( s e e s e c t i o n on P a l l a d i u m

3 3 4

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M e t a l s f o r p r e p a r a t i o n ) , w h i c h i s i n s e r t e d into a s m a l l t u b u l a r e l e c t r i c f u r n a c e . At m a x i m u m l i n e v o l t a g e , t h e f u r n a c e s h o u l d

r e a c h about 350°C a n d at m o s t 400°C.

+ T h e f u r n a c e a s w e l l a s t h e adjoining w a s h t o w e r c o n t a i n i n g c o n c e n t r a t e d

H2S 04 s h o u l d b e fixed to t h e g l a s s c y l i n d e r w i t h c o l l a r s m a d e of t h i c k Al s h e e t . T h i s a p p a r a t u s w o r k s b e s t w h e n a u n i f o r m s t r e a m of v e r y p u r e 02 i s n e e d e d .

If it i s d e s i r e d t o know a c c u r a t e l y t h e q u a n t i t i e s of p r o d u c t s and r e - a c t a n t s , a s e c o n d e l e c t r o l y z e r of t h e s a m e t y p e i s c o n n e c t e d in s e r i e s with t h e f i r s t , a n d t h e Os e v o l v e d in t h e l a t t e r i s c o l l e c t e d in s u i t a b l e g l a s s b u r e t t e s ; i . e . , t h e s e c o n d a p p a r a t u s i s u s e d a s a c o u l o m e t e r . A l s o , any d e - s i r e d m i x t u r e with H2 m a y b e p r e - p a r e d by a t t a c h i n g u n d e r t h e b e l l a s e c o n d a u x i l i a r y e l e c t r o d e c o n n e c t e d in p a r a l l e l with t h e c a t h o d e t h r o u g h a F i g . 150. E l e c t r o l y t i c r e s i s t a n c e . T h e p a l l a d i u m a s b e s t o s p r e p a r a t i o n of o x y g e n t ub e i g th e n o m i t t e d > o f C O Ur s e . By

o r h y d r o g e n . s u i t a b l e c h o i c e of t h e r e s i s t a n c e , any d e s i r e d m i x t u r e of 02 a n d H2 c a n b e r e a d i l y o b t a i n e d . T h e a u x i l i a r y e l e c t r o d e i s i n s u l a t e d by a g l a s s U t u b e a n d i s i n t r o d u c e d into t h e b e l l f r o m b e l o w .

Given t h e a b o v e d i m e n s i o n s , t h e a p p a r a t u s c a n c a r r y a c u r r e n t of about 5 a m p . and f u r n i s h about o n e l i t e r of oxygen p e r h o u r . W i t h p r o l o n g e d high c u r r e n t , t h e KOH of t h e e l e c t r o l y t e u n d e r t h e b e l l i s o c c a s i o n a l l y d e p l e t e d , r e s u l t i n g in p r o n o u n c e d c o r r o s i o n of t h e a n o d e . If t h e e l e c t r o l y t e b e c o m e s d a r k , it m u s t b e r e m i x e d , w h i c h c a n b e e a s i l y done by a l l o w i n g it t o r i s e in t h e b e l l . Caution: the poles may not be interchanged during the run! An o x y h y d r o g e n g a s e x p l o s i o n , w h i c h i s t h e n u n a v o i d a b l e , c a n h a v e v e r y s e r i o u s c o n s e q u e n c e s b e c a u s e of t h e c o n c e n t r a t e d p o t a s s i u m h y d r o x i d e s o l u t i o n . F o r t h i s r e a s o n , c a r e f u l c h e c k i n g of t h e c o r r e c t p o l e c o n n e c t i o n s i s i n d i s p e n s a b l e , e v e n d u r i n g t h e c h e c k - o u t r u n .

O t h e r m o d i f i c a t i o n s of e l e c t r o l y z e r s , w h i c h y i e l d v e r y p u r e Oa, h a v e b e e n d e s c r i b e d by P a n e t h a n d by B r a u e r . F o r t h e r e m o v a l of t h e l a s t t r a c e s of finely d i s p e r s e d d r o p l e t s f r o m t h e e l e c t r o - l y t i c a l l y p r o d u c e d g a s , s e e H. L u x .

II. OXYGEN BY CATALYTIC DECOMPOSITION OF HYDROGEN PEROXIDE

An e x c e l l e n t a p p a r a t u s f o r t h e c o n t i n u o u s p r o d u c t i o n of f a i r l y l a r g e q u a n t i t i e s of v e r y p u r e oxygen h a s b e e n d e s c r i b e d by

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F i g . 1 5 1 . P r e p a r a t i o n of o x y g e n f r o m h y d r o ­

g e n p e r o x i d e . Von W a r t e n b e r g . T h e h a l f - l i t e r c a l i b r a t e d f l a s k A ( F i g . 151) i s c l o s e d off with a g r o u n d g l a s s a d a p t e r Β w h i c h i s s e a l e d with o r d i n a r y s t o p c o c k g r e a s e . T h i s a d a p t e r i s p r o v i d e d with a s m a l l g l a s s w i n c h (7, f r o m w h i c h a t h i n s p i r a l

of Ni s h e e t i s s u s p e n d e d by a t h i n P t w i r e . T h e 6 X 7 c m . Ni s h e e t i s p l a t i ­ n i z e d in t h e s a m e way a s t h e e l e c t r o d e s of a conductivity c e l l and i s ignited at dull r e d h e a t in a H2 s t r e a m u n t i l it b e c o m e s light g r a y . B e f o r e t h e f i r s t r u n , it i s a l l o w e d to r e a c t i n 3 0 % H2O2 for s o m e t i m e . T h i s r e m o v e s t h e l o o s e P t p a r t i c l e s . Without t h i s t r e a t m e n t , t h e d e c o m p o s i t i o n of H20 would c o n ­ t i n u e e v e n a f t e r t h e c e s s a t i o n of t h e r u n and it would a l s o c a u s e p r e m a t u r e c o n s u m p t i o n of t h e H302 in t h e a p ­ p a r a t u s . T h e g r o u n d g l a s s a d a p t e r a l s o c o n t a i n s a few g l a s s b e a d s w h i c h r e t a i n t h e c o a r s e liquid s p r a y . A s m a l l p r e s s u r e r e l e a s e v a l v e c o n t a i n - t a i n i n g Hg i s c o n n e c t e d at F. A s i x - c m . long p l a t i n i z e d Cu w i r e s c r e e n i s p l a c e d in t h e v e r t i c a l t u b e a t t a c h e d

p a s t s t o p c o c k Η in o r d e r to d e c o m p o s e t h e l a s t t r a c e s of e n t r a i n e d h y d r o g e n p e r o x i d e . A s m a l l r o t a m e t e r i s a t t a c h e d a f t e r t h e s p i r a l w a s h f l a s k c o n t a i n i n g c o n c e n t r a t e d H3S 04. If t h e a p p a r a t u s i s t o b e o p e r a t e d for a long t i m e , it i s p l a c e d in a l a r g e c o n t a i n e r full of c o l d w a t e r to r e m o v e t h e h e a t d e v e l o p e d d u r i n g t h e r u n . After a s h o r t s t a r t u p p e r i o d , t h e g a s e s d i s s o l v e d in t h e liquid a r e d i s p l a c e d a n d v e r y p u r e , H202- f r e e g a s i s p r o d u c e d . C o m m e r i c a l P e r h y d r o l i s u s e d a s s t a r t i n g m a t e r i a l . With t h i s m a t e r i a l , t h e p o s t evolution of 03 i s r e d u c e d in c o m p a r i s o n with v e r y p u r e P e r h y d r o l . T h e d e s i r e d r a t e of evolution i s a d j u s t e d by i n c r e a s i n g o r d e c r e a s i n g t h e s u b m e r g e d s u r f a c e of t h e Ni s h e e t , u s i n g t h e g l a s s w i n c h . T h e evolution of g a s s u b s i d e s only a f t e r t h e c o n ­ c e n t r a t i o n of H3Os d r o p s to about 1.5%. Half a l i t e r of 30% H3Os y i e l d s about 45 l i t e r s of 03.

A Kipp g e n e r a t o r c a n a l s o b e u s e d f o r oxygen p r o d u c t i o n . In t h i s c a s e , 3% H3Os i s u s e d and t h e g e n e r a t o r i s c h a r g e d with c u b e s m a d e of M n 03 a n d a b i n d e r .

A c c o r d i n g to Von W a r t e n b e r g , v e r y s m a l l q u a n t i t i e s of Ο3 in i n e r t g a s e s c a n b e d e t e c t e d m o s t s i m p l y by m e a n s of a b e a d of w h i t e p h o s p h o r u s . T h e r i s i n g v a p o r s t r e a k s of P302 i n d i c a t e a s l i t t l e a s 0.002 v o l . % of Os, p r o v i d e d no g a s e s w h i c h i n t e r f e r e w i t h t h e oxidation ( H2S , S 02, h a l o g e n s , N304, CaH4, etc.) a r e p r e s e n t [Z. E l e k t r o c h e m . 36, 296 (1930)]. Von W a r t e n b e r g h a s a l s o

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d e s c r i b e d a s i m p l e a p p a r a t u s f o r d e t e c t i n g 02 in t h i s m a n n e r [Chem. Ing. T e c h n . 2<6, 418 (1954)]. T h i s a p p a r a t u s m a y b e u s e d at a m o m e n t ' s n o t i c e .

PROPERTIES:

F o r m u l a weight 3 2 . 0 0 0 . C o l o r l e s s , o d o r l e s s g a s . C o n d e n s e s to a b l u i s h l i q u i d . M . p . —218.4°C, b . p . - 1 8 3 . 0 ° C . C r i t . t . - 1 1 8 . 8 ° C . C r i t . p . 49.7 a t m . d ( - 1 8 3 ° C ) 1.134. W e i g h t p e r l i t e r (0°C, 760 m m . ) 1.429 g.

REFERENCES:

A. K l e m e n c . B e h a n d l u n g und R e i n d a r s t e l l u n g d e r G a s e [ T r e a t m e n t and P u r i f i c a t i o n of G a s e s ] , 2nd Ed., Vienna, 1 9 4 8 .

H. von W a r t e n b e r g . Z . a n o r g . a l l g . C h e m . 2 3 8 , 297 (1938).

F . P a n e t h and R. P e t e r s . Z . p h y s . C h e m . 134, 365 (1928).

G. B r a u e r . Z. a n o r g . C h e m . 2 5 5 , 105 (1947).

V. I. S h e m y s h y n . K h i m . Shkola No. 6, 5 7 - 5 8 ; a b s t r a c t in C h e m . Z e n t r . 54, 8172.

H. L u x . Z. E l e k t r o c h e m . 4 8 , 213 (1942).

Ozon e o3

T h e o z o n i z e r ( F i g . 152), t h e p r i n c i p l e of w h i c h w a s d e s c r i b e d by S i e m e n s a n d B e r t h e l o t , i s s t i l l t h e m o s t s u i t a b l e a p p a r a t u s for t h e p r e p a r a t i o n of o z o n e . F o u r o r s i x o z o n e t u b e s a r e c o n n e c t e d in s e r i e s a n d p l a c e d t o g e t h e r in a g l a s s c y l i n d e r .filled with d i l u t e C u S 04 s o l u t i o n , w h i c h s e r v e s a s t h e e x t e r n a l e l e c t r o d e . T h e g l a s s c y l i n d e r i s about 3 0 - 4 0 c m . high. T h e o z o n e t u b e s a r e m a d e of t h i n - w a l l soft g l a s s , a s u n i f o r m a s p o s s i b l e . ( T h e a u t h o r h a s o b s e r v e d on o c c a s i o n t h a t P y r e x o z o n e t u b e s a r e not a s effective a s t h o s e of soft g l a s s . ) T h e i n n e r t u b e h a s a d i a m e t e r of 10 to 12 m m . and i s fused c o n c e n t r i c a l l y t o t h e o u t e r t u b e . T h r e e s m a l l g l a s s b e a d s on t h e i n n e r t u b e k e e p it in t h e c o r r e c t p o s i t i o n . T h e p o s i t i o n i n g of t h e i n n e r t u b e by i n d e n t a t i o n s in t h e o u t e r t u b e should b e a v o i d e d . Such i n d e n t a t i o n s d e c r e a s e t h e d i s t a n c e b e t w e e n t h e i n n e r and o u t e r e l e c t r o d e . T h e c o n s e q u e n t h i g h e r e l e c t r i c field d e n s i t y at t h e s e p o i n t s r e s u l t s in b r e a k d o w n s , l e a d i n g to t h e d e s t r u c t i o n of t h e t u b e . T h e d i s t a n c e b e t w e e n t h e two t u b e s , i . e . , t h e a i r g a p b e t w e e n t h e m , i s about 1 m m . T h e individual t u b e s a r e fused t o g e t h e r in p a i r s , t h e fusion point b e i n g at t h e b o t t o m . Two p a i r s a r e a l w a y s c o n n e c t e d w i t h e a c h o t h e r a t t h e t o p . In t h i s way t h e 02 s t r e a m e n t e r s t h e f i r s t o z o n e t u b e a t t h e t o p and a l s o l e a v e s

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220 ν

F i g . 152. P r e p a r a t i o n of o z o n e ( o z o n i z e r ) . A ) flow m e t e r ; B) a n a l y s i s v e s s e l w i t h d e c o m p o s i t i o n d e v i c e for o z o n e ; 0) r e a c t i o n v e s s e l ; D) t u b e with g l a s s f r a g m e n t s a n d c o n ­

c e n t r a t e d KOH solution for d e c o m p o s i n g e x c e s s o z o n e . t h e l a s t t u b e at t h e t o p . T h e i n n e r t u b e s a r e filled with C u S 04 s o l u t i o n to a l e v e l s o m e w h a t h i g h e r t h a n t h a t in t h e c y l i n d e r s . Thin w i r e s of s t a i n l e s s s t e e l 304 a r e u s e d a s e l e c t r i c a l l e a d s . C o r k s t o p p e r s p r e v e n t e v a p o r a t i o n of t h e s o l u t i o n . T h e individual w i r e s a r e i n t e r c o n n e c t e d . T h e a s s e m b l y i s t h e n c o n n e c t e d to o n e p o l e of a s m a l l t r a n s f o r m e r ^ ( s o - c a l l e d i n s t r u m e n t t r a n s f o r m e r ) w h i c h g i v e s about 8000 v o l t s a t t h e s e c o n d a r y . T h e o t h e r p o l e of t h e t r a n s f o r m e r i s g r o u n d e d and i s c o n n e c t e d w i t h t h e o u t e r l a y e r — t h e s o l u t i o n in t h e c y l i n d e r — b y a n i m m e r s e d w i r e . When a 5 0 0 -

c y c l e a l t e r n a t i n g c u r r e n t i s a v a i l a b l e , it s h o u l d b e u s e d in p r e f e r e n c e t o t h e 6 0 - c y c l e supply s i n c e h i g h e r o z o n e c o n c e n t r a t i o n s a r e t h e n o b t a i n e d . C y l i n d e r Os i s u s e d a s t h e s t a r t i n g m a t e r i a l . It i s d r i e d with c o n c e n t r a t e d H2S 04 and i t s flow c o n t r o l l e d by m e a n s of flow m e t e r A. If t h e p r e s e n c e of n i t r o g e n o x i d e s in t h e p r o d u c t i s u n ­ d e s i r a b l e , e l e c t r o l y t i c oxygen s h o u l d b e u s e d a s t h e r a w m a t e r i a l .

D e t e r m i n a t i o n of t h e o z o n e c o n c e n t r a t i o n , w h i c h i s i n d i s p e n s a b l e in m a n y s t u d i e s , c a n b e c a r r i e d out by p a s s i n g t h e g a s t h r o u g h a KI s o l u t i o n c o n t a i n i n g s o m e s o l i d b o r i c a c i d . T h e iodine f o r m e d a c c o r d i n g t o t h e e q u a t i o n :

03 + 2 KI + H20 = I2 + 2 KOH + 02

i s t i t r a t e d with 0.1 Ν t h i o s u l f a t e .

A m u c h q u i c k e r p r o c e d u r e , w h i c h i s sufficiently a c c u r a t e for m o s t p u r p o s e s , i s b a s e d on t h e v o l u m e i n c r e a s e a s s o c i a t e d with

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t h e d e c o m p o s i t i o n of o z o n e a c c o r d i n g to t h e e q u a t i o n

2 03 = 3 02

T h e s e t u p f o r t h i s d e t e r m i n a t i o n i s shown s c h e m a t i c a l l y in F i g . 152 (B).

T h e t w o - w a y s t o p c o c k #x a l l o w s t h e g a s to flow e i t h e r into a n a l y s i s v e s s e l Β o r into r e a c t i o n v e s s e l 0. It i s b e s t to l u b r i c a t e it w i t h P2Ob, w h i c h i s t h e n c o n v e r t e d t o H P 03. To p r e v e n t too r a p i d l i q u e f a c t i o n of t h e a c i d (which would p r o d u c e a l e a k ) , o r d i n a r y s t o p c o c k g r e a s e i s a p p l i e d a t t h e t o p and b o t t o m r i m of t h e s t o p ­ c o c k . S t o p c o c k s w h i c h c l o s e a t t h e b o t t o m a r e a l s o v e r y u s e f u l . All o t h e r s t o p c o c k s in t h e a p p a r a t u s c a n b e s e a l e d with o r d i n a r y s t o p c o c k g r e a s e .

T h e a n a l y s i s v e s s e l Β i s c y l i n d r i c a l . It c o n t a i n s a t h i n s p i r a l of P t w i r e s u p p o r t e d by two s e a l e d - i n c u r r e n t l e a d s . T h e w i r e g l o w s w h e n t h e c u r r e n t f r o m a s m a l l l i n e t r a n s f o r m e r i s p a s s e d t h r o u g h it. T h e a n a l y s i s v e s s e l i s c o n n e c t e d v i a s t o p c o c k ff3 w i t h a n H2S 04 m a n o m e t e r M. Stopcock H3 i s c o n n e c t e d t o t h e hood t h r o u g h t u b e D9 w h i c h w i l l b e d i s c u s s e d l a t e r . T h e a n a l y s i s v e s s e l i s p l a c e d in a w a t e r b a t h , w h i c h m u s t b e l a r g e enough t o p r e v e n t t e m p e r a t u r e f l u c t u a t i o n s d u r i n g t h e m e a s u r e m e n t (the b a t h t e m p e r a t u r e m a y b e c h e c k e d w i t h a t h e r m o m e t e r ) .

T h e r u n p r o c e e d s a s f o l l o w s : T h e e n t i r e a p p a r a t u s i s f i r s t f l u s h e d with 02, s t o p c o c k # \ i s t u r n e d t o w a r d t h e a n a l y s i s v e s s e l , a n d v o l t a g e i s a p p l i e d t o t h e o z o n i z e r . (A r e d c o n t r o l l a m p L c o n ­ n e c t e d in p a r a l l e l w i t h t h e p r i m a r y of t h e t r a n s f o r m e r i s highly r e c o m m e n d e d . ) T h e flow r a t e i s t h e n a d j u s t e d by m e a n s of flow m e t e r A and t h e a p p a r a t u s i s f l u s h e d f o r s o m e t i m e . Stopcock ff1 i s t h e n t u r n e d t o w a r d 09 and H3 i s c l o s e d . A f t e r t h e z e r o p o s i t i o n h a s b e e n a d j u s t e d on t h e m a n o m e t e r , #2 i s a l s o c l o s e d . T h e h e a t i n g c u r r e n t f o r t h e P t w i r e i s t u r n e d on f o r a few m i n u t e s , and a f t e r t h e h e a t i n g c u r r e n t h a s b e e n t u r n e d off, ff2 i s a g a i n o p e n e d . T h e r e a d i n g i s t a k e n w h e n t h e m a n o m e t e r l e v e l c e a s e s t o c h a n g e . T h e h e a t i n g p r o c e s s i s r e p e a t e d t o m a k e c e r t a i n t h a t a l l t h e o z o n e h a s b e e n d e c o m p o s e d . T h e o z o n e c o n t e n t of t h e g a s c a n b e d e t e r ­ m i n e d f r o m t h e v o l u m e i n c r e a s e o r p r e s s u r e i n c r e a s e g i v e n by t h e p r e v i o u s l y c i t e d e q u a t i o n . T h e m a n o m e t e r m a y b e c a l i b r a t e d d i r e c t l y in p e r c e n t o z o n e . T h e r e l i a b i l i t y of t h e a n a l y z e r i s c h e c k e d by t h e i o d o m e t r i c m e t h o d . T h e o z o n e f r o m t h e r e a c t i o n v e s s e l i s v e n t e d into t h e hood t h r o u g h t u b e D9 filled w i t h g l a s s f r a g m e n t s . T h e g l a s s f r a g m e n t s a r e w e t t e d with c o n c e n t r a t e d K O H s o l u t i o n , w h i c h c o m p l e t e l y d e c o m p o s e s t h e o z o n e .

T h i s d e v i c e i s m u c h s a f e r t h a n t h e f r e q u e n t l y u s e d h e a t e d t u b e s in w h i c h t h e s o l v e n t v a p o r s f r o m t h e r e a c t o r m a y a c c u m u l a t e . If m i x e d w i t h oxygen, t h e y o c c a s i o n a l l y i g n i t e and g i v e r i s e t o v i o l e n t e x p l o s i o n s .

(7)

It i s b e s t to p l a c e t h e e n t i r e a p p a r a t u s u n d e r a hood, with t h e t r a n s f o r m e r s and t h e o z o n i z e r p r o p e r b e i n g e n c l o s e d in s e p a r a t e b o x e s . At t h e v e r y l e a s t t h e e l e c t r i c a l c o m p o n e n t s s h o u l d b e p r o ­ t e c t e d f r o m c o n t a c t with o z o n e .

T h e p r e s e n t a p p a r a t u s will y i e l d an oxygen s t r e a m w i t h a n o z o n e c o n c e n t r a t i o n of 10-12%, e s p e c i a l l y if 5 0 0 - c . p . s . AC i s u s e d . Still h i g h e r c o n c e n t r a t i o n s c a n b e o b t a i n e d by c o o l i n g t h e o z o n i z e r . To obtain a c o n s t a n t 03 c o n t e n t in t h e g a s , G r e e n w o o d s u g g e s t s cooling of t h e i n n e r t u b e of t h e o z o n i z e r t o a c o n s t a n t t e m p e r a t u r e .

PROPERTIES:

C o l o r l e s s g a s , b l u e in l a r g e v o l u m e s ; c h a r a c t e r i s t i c u n p l e a s a n t o d o r . Deep b l u e liquid. E x t r e m e l y d e l e t e r i o u s to t h e h e a l t h , p a r t i c u l a r l y in h i g h e r c o n c e n t r a t i o n s . B . p . — 1 1 2 . 3 ° C , m . p . —251°C.

C r i t . t . —5°C. d (—183°C) 1.78. D e c o m p o s e s r u b b e r c o m p l e t e l y in a few m i n u t e s .

REFERENCES:

F . R. G r e e n w o o d . Ind. E n g . C h e m . , A n a l . E d . 17, 4 4 6 - 4 4 7 (1945).

E . D. B o e l t e r , G. L. P u t n a m and Ε . I. C a s h ( I o d o m e t r i c Ozone D e t e r m i n a t i o n ) . Analyt. C h e m . 22, 1 5 3 3 - 1 5 3 5 .

E . B r i n e r , V. S p r e t e r and B, K o v a l i v . Bull. S o c C h i m . B e i g e 6 2 , 5 5 - 6 6 (1953).

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