UBC Theses and Dissertations

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UBC Theses and Dissertations

The heats of combustion of the cis and trans isomers of decahydronapthalene Gould, Leslie Robert 1938

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T h e H e a t s o f C o m b u s t i o n o f t h e C i s a n d T r a n s I s o m e r s o f D e o a h y d r o n a p h t h a l e n e . A T h e s i s S u b m i t t e d f o r t h e D e g r e e o f M a s t e r o f A p p l i e d . S c i e n c e i n t h e D e p a r t m e n t o f C h e m i s t r y . T h e U n i v e r s i t y o f B r i t i s h C o l u m b i a t>y L e s l i e R. G o u l d A p r i l , Table of Contents . Page P a r t I . Separat ion of Ois and Trans Becahydronaphthalene Introduct ion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 iU Reasons 1 f o r research 1 Separat ion by R e c t i f i c a t i o n . . . . . . . . . . . . . . « . . . . . . . . . . . . . . . . . . . . 2 '• A* D e s c r i p t i o n of. apparatus '.>'•;•••« 2 Bo Procedure fo l lowed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 C. Results 3 P u r i f i c a t i o n by F r a c t i o n a l Crystallization ..................... 7 A* D e s c r i p t i o n of apparatus and procedure . . . . . . . . . . . . . . . 8 B. Determinat ion©f f r e e z i n g p o i n t s . . . . . . . . . . . . . . . . . . . . . 8 C. Resu l t s 9 Part I I . The Heats of'Combustion o f the Isomers of Decahydronaphthalene.. Apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 A» Reasons f o r choice . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 B. Application of standard bomb ca lor imeter . . . . . . . . . . . . . 11 C> Method o f s tandard iz ing equipment . . . . . . . . . . . . . . . . . . . . 14 Experimental Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . IS 'Calculations .................................. '••................ I? A® Method used t o c a l c u l a t e c o o l i n g correction 17 B. R e s u l t s . . . . . . . . . . . . . . . « , « , . „ » . „ « . . . . . « . . . . . . . . . . 19 C . C a l c u l a t i o n o f heat capac i ty of bomb . . . . . . . . . . . . . . . . . 20 9*. C a l c u l a t i o n o f heat of combustion > ' : . . - . ' . * . . . . . . . . . . . . . . . 21 D iscuss ion of Results „ 21 Bibl iography . . . . . . . . . . . . . . . . . . . . . . . . . 23 P a r t I . S e p a r a t i o n o f t h e P u r e G i s a n d T r a n s I s o m e r s o f D e c a a y d r o n a p h t h a l e n e I n t r o d u c t i o n A . R e a s o n s f o r r e s e a r c h U n d e r t h e d i r e c t i o n o f D r . W. S 1. S e y e r c o n s i d e r a b l e w o r k h a s b e e n d o n e at t h i s i n s t i t u t i o n on a s t u d y o f t h e i s o m e r i c f o r m s o f d e c a h y d r o n a p h t h a 1 e n e . D e o a h y d r o n a p h t h a l e n e i s b e l i e v e d t o e x i s t i n f i v e s t e r e o - i s o m e r i c f o r m s . Two o f t h e s e f o r m s a r e c o n s i d e r e d t o b e l i m i t i n g p o s i t i o n s o f t h e o t h e r t h r e e a n d as a r e s u l t a r e o f g r e a t e r s t a b i l i t y . The w o r k o f R. D. W a l k e r ^ - ^ p r o v e d c o n c l u s i v e l y t h e p r e s e n c e o f two i s o m e r s . T h e s e two i s o m e r s w h i c h h a v e q u i t e d i f f e r e n t p r o p e r t i e s a r e known a s " c i s " a n d " t r a n s " . I n 1 9 3 6 - ' 3 7 t h e f i r s t s u c c e s s f u l s e p a r a t i o n o f t h e o i s and t r a n s i s o m e r s was a c c o m p l i s h e d by D r . W. J 1 . S e y e r and R. D. W a l k e r . ^ ^ T h e s e i n v e s t i g a t o r s , b y f r a c t i o n a l d i s -t i l l a t i o n u n d e r r e d u c e d p r e s s u r e , o b t a i n e d two f r a c t i o n s , o n e o f h i g h c i s c o n t e n t and t h e o t h e r o f h i g h t r a n s . Then b y a l e n g t h y p r o c e s s o f f r a c t i o n a l c r y s t a l l i z a t i o n p u r e c i s a n d ( 1 ) W a l k e r , R. D . , M . A . S c . T h e s i s , 1 9 3 7 . •(E) I b i d . t r a n s was o b t a i n e d . The o b j e c t o f t h i s r e s e a r c h was t w o - f o l d , f i r s t to s e p a r a t e m o r e c i s a n d t r a n s d e c a l i n b y t h e m e t h o d o u t l i n e d a b o v e , a n d t h e n t o d e t e r m i n e t h e h e a t s o f c o m b u s t i o n o f t h e two i s o m e r s . S e p a r a t i o n b y R e c t i f i c a t i o n A . D e s c r i p t i o n o f a p p a r a t u s The a p p a r a t u s u s e d was t h a t u s e d b y R. D. W a l k e r a n d shown i n f i g u r e 1 . The s t i l l was a 3000 c . c . d i s t i l l i n g f l a s k a n d was e q u i p p e d w i t h a 95 i n c h r e c t i f y i n g c o l u m n p a c k e d w i t h #18 j a c k c h a i n . S l i g h t c h a n g e s w e r e made i n t h e a p p a r a t u s to i m p r o v e i t s o p e r a t i o n . To g i v e more c o n s t a n t r a t e o f h e a t i n g o f t h e s t i l l t h e g a s b u r n e r o r i g i n a l l y u s e d was r e p l a c e d b y an e l e c t r i c h e a t e r w h i c h c o u l d s u p p l y e n e r g y u p to 600 w a t t s . The h e a t e r was d e s i g n e d so t h a t i t f i t t e d t h e b o t t o m o f t h e d i s t i l l i n g f l a s k . The c a p i l l a r y p r e v i o u s l y u s e d was r e p l a c e d by one o f much s m a l l e r b o r e so t h a t t h e r a t e o f p r o d u c t drawn o f f was r e d u c e d f r o m a b o u t 115 c . c . p e r h o u r t o 10 - I E c . c . p e r h o u r . I n t h i s way a mueh b e t t e r s e p a r a t i o n was o b t a i n e d on e a c h r u n . B . P r o c e d u r e f o l l o w e d I t was f o u n d t h a t i n t h e r a w d e c a l i n s u p p l i e d by t h e E a s t m a n K o d a k G o . t h e r e was a c o n s i d e r a b l e amount o f i m p u r i t y w h i c h c o u l d be r e m o v e d by washing- w i t h c o n c e n t r a t e d s u l p h u r i c a c i d . H e n c e t h e raw d e c a l i n was w a s h e d w i t h a c i d u n t i l t h e wash a c i d was no l o n g e r c o l o u r e d , t h e n w i t h a l y e s o l u t i o n , low P££5su#£ RECTIFICATION COL UMN. and f i n a l l y w i t h w a t e r u n t i l n e u t r a l . The s t i l l was c h a r g e d w i t h a known q u a n t i t y o f t h e m a t e r i a l , u s u a l l y 2000 c . c . a n d , a f t e r t h e d e s i r e d p r e s s u r e , 10 mm* o f m e r c u r y , h a d b e e n r e a c h e d , t h e h e a t i n g was s t a r t e d . When d i s t i l l a t i o n h a d b e g u n 13 v o l t s w e r e a p p l i e d t o t h e h e a t i n g c o i l s on t h e c o l u m n . T h e s e c o i l s were u s e d t o o b t a i n a d i a b a t i c o p e r a t i o n a n d were r u n a t a l o w e r v o l t a g e t h a n t h a t u s e d b y W a l k e r s i n c e i t was f o u n d t h a t d i s t i l l a t i o n i n t h e c o l u m n was t a k i n g p l a c e . , The r a t e o f r e f l u x was c o n t r o l l e d by t h e r a t e o f h e a t i n g o f t h e s t i l l and was j u d g e d by t h e amount o f m a t e r i a l f l o w i n g b a c k down t h e c o l u m n . A s t h e a v e r a g e t e m p e r a t u r e o f t h e c o l u m n r o s e t h e v o l t a g e on t h e h e a t i n g c o i l s was i n c r e a s e d t o 16 v o l t s . T h e t i m e o f c h a n g i n g f r o m one p r o d u c t r e s e r v o i r . t o t h e n e x t was j u d g e d by t h e o v e r h e a d t e m p e r a t u r e o f t h e c o l u m n . T h e d i s t i l l a t i o n was d i s c o n t i n u e d when t h e c o l u m n t e m p e r a t u r e r o s e r a p i d l y . T h i s r i s e was due t o t h e d i s t i l l a t i o n o f h e a v y e n d s f r o m t h e s t i l l . 0 . R e s u l t s The r e s u l t s o f t h e r e c t i f i c a t i o n a r e shown i n t a b l e I . T a b l e I . R e c t i f i c a t i o n # 1 . C h a r g e - 2000 c . c . E a s t m a n K o d a k d e c a l i n , a c i d washed n e u t r a l i z e d a n d d r i e d . n j n = 1 . 4 7 9 6 5 ( 1 3 $ T r a n s ) D^n = 0 . 8 9 2 0 P r e s s u r e i n A p p a r a t u s - 10 mm. o f H g . o C o n d e n s e r w a t e r - A p p r o x i m a t e l y c o n s t a n t a t 20 C . R e s u l t s F r a c t i o n 1 2 3 4 5 V o l u m e ( c . c . ) 121 332 743 352 290 n D „ 1 . 4 7 0 8 1 1 . 4 7 1 7 0 1 . 4 7 9 7 5 1 . 4 8 1 1 3 1 . 4 8 2 2 9 20 fo T r a n s 91 82 IB 0 % O i s 9 18 88 100 R e c t i f i c a t i o n # 2 . C h a r g e - £025 c . c . E a s t m a n K o d a k d e c a l i n - a c i d w a s h e d , n e u t r a l i z e d and d r i e d . n ^ Q = 1 . 4 7 6 9 5 ( 1 3 $ t r a n s ) = 0 . 8 9 2 0 P r e s s u r e i n a p p a r a t u s - 10 mm. H g . C o n d e n s e r w a t e r - o o n s t a n t a t 2 0 ° 0 . R e s u l t s F r a c t i o n 1 2 3 4 5 V o l u m e ( c . c ) 225 240 745 4 0 3 n ^ 0 1 . 4 7 0 7 6 1 . 4 7 4 5 5 1 . 4 8 0 9 8 1 . 4 8 2 8 3 fo T r a n s 92 57 3 °h Ois, 8 4 3 97 R e c t i f i c a t i o n # 5 . , C h a r g e - 1755 c c . made u p o f f r a c t i o n s #4 and #5 o f r e c t i f i c a t i o n #1 a n d f r a c t i o n s #3 and #4 o f r e c t i f i c a t i o n # 2 . n | Q = 1*48166 . P r e s s u r e i n a p p a r a t u s - 10 mm. H g . C o n d e n s e r w a t e r - c o n s t a n t a t 2 0 ° C . R e s u l t s F r a c t i o n 1 2 3 4 5 Vo lume ( c . c . ) 162 4 2 3 54Q 203 114 n D 1 . 4 8 0 2 4 1 , 4 8 1 0 8 1 . 4 8 1 1 3 1 , 4 8 1 1 8 1 . 4 8 1 1 8 20 <fo T r a n s 7 . 5 0 0 0 0 % O i s 9 2 . 5 100 100 100 100 R e c t i f i c a t i o n # 4 . C h a r g e - 1490 c . c . - made u p o f f r a c t i o n s #1 a n d #2 o f r e c t i f i c a t i o n # 1 , f r a c t i o n s #1 and #2 o f r e c t i f i c a t i o n #2, a n d 572 c . c . o f h i g h t r a n s c o n t e n t f r o m W a l k e r s w o r k ( a c i d w a s h e d ) . n g 0 = 1 . 4 6 8 8 3 P r e s s u r e i n a p p a r a t u s - 10 mm. H g . C o n d e n s e r w a t e r - c o n s t a n t at 2 0 ° C . 6 . R e s u l t s F r a c t i o n 1 2 3 4 5 V o l u m e ( o . o . ) 230 4 9 0 240 195 141 • r r 0 1 , 4 6 1 9 2 1 , 4 6 9 1 8 1 . 4 6 9 5 8 1 . 4 6 9 6 8 1 . 4 7 1 0 0 fo T r a n s — — - 100 100 100 fo C i s - . — 0 0 0 N o t e ; The f r a c t i o n s o f t h i s r e c t i f i c a t i o n , w e r e f o u n d u n s a t i s f a c t o r y s i nee a c o n s t a n t f r e e z i n g p o i n t c o u l d n o t h e o b t a i n e d on a n u m b e r o f r e c r y s t a l i i z a t i o n s . R e c t i f i c a t i o n $ 5 . C h a r g e - 2000 c . c . u n w a s h e d E a s t m a n K o d a k C o . d e c a l i n . P r e s s u r e i n a p p a r a t u s - 10 mm. H g . C o n d e n s e r w a t e r - c o n s t a n t at 2 0 ° C . R e s u l t s F r a c t i o n 1 2 3 4 5 V o l u m e ( c . c * ) 288 135 140 173 92 n ^ Q 1 . 4 6 9 3 8 1 . 4 6 9 5 8 1 . 4 6 9 8 3 1 . 4 7 1 5 0 1 . 4 7 7 6 0 fo T r a n s 100 98 84 31 fo C i s — 0 2 16 69 R e c t i f i c a t i o n # 6 . C h a r g e - 1380 c . c . E a s t m a n K o d a k C o . d e c a l i n and 900 c . c . o f 90fo t r a n s f r o m r e c t i f i c a t i o n # 5 . P r e s s u r e i n a p p a r a t u s - 10 mm. H g . C o n d e n s e r w a t e r - c o n s t a n t a t 2 0 ° C . 7 . R e s u l t s F r a c t i o n 1 2 3 4 5 V o l u m e ( c . c . ) 325 180 320 4 1 380 n ? 1 . 4 6 8 9 8 1 . 4 6 9 6 8 1 . 4 6 9 6 8 1 . 4 6 9 6 8 1 . 4 6 9 8 7 io T r a n s - - - 100 100 100 99 % O i s - — 0 . 0 0 1 R e c t i f i c a t i o n # 7 . C h a r g e - F r o m r e c r y s t a l l i z a t i o n s o f r e c t i f i c a t i o n s #5 a n d # 6 . P r e s s u r e i n a p p a r a t u s - 10 mm. o f H g . o C o n d e n s e r w a t e r - c o n s t a n t a t 20 0 . R e s u l t s F r a c t i o n 1 2 3 4 5 n g 0 1 . 4 6 9 0 8 1 . 4 6 9 5 3 1 . 4 6 9 5 8 1 . 4 6 9 5 3 1 . 4 6 9 5 3 fo T r a n s 100 100 100 100 $ C i s — 0 0 0 0 P u r i f i c a t i o n b y F r a c t i o n a l C r y s t a l l i z a t i o n I t was f o u n d t h a t t h e r e was a l i m i t t o t h e p u r i t y o f t h e p r o d u c t t h a t c o u l d b e o b t a i n e d b y r e c t i f i c a t i o n a n d f r a c t i o n a l c r y s t a l l i z a t i o n was u s e d t o g i v e t h e p u r e i s o m e r s . B e c a u s e o f t h e h i g h p u r i t y o f t h e c i s f r a c t i o n s no d i f f i c u l t y was e x p e r i e n c e d i n o b t a i n i n g t h e p u r e i s o m e r . I n t h e c a s e o f t h e t r a n s a g r e a t many m o r e c r y s t a l l i z a t i o n s w e r e n e c e s s a r y , •8. A . D e s c r i p t i o n o f a p p a r a t u s and p r o c e d u r e The f r a c t i o n s f r o m t h e s t i l l h i g h i n e i t h e r i s o m e r w e r e c o m b i n e d and p l a c e d i n a l a r g e dewar f l a s k h o l d i n g a b o u t 500 c . c . T h i s was p l a c e d i n a l a r g e r dewar and t h e s p a c e b e t w e e n t h e two p a c k e d w i t h d r y i c e . The f i r s t f l a s k was e m p l o y e d t o g i v e a l o w h e a t t r a n s f e r c o e f f i c i e n t . A p l a t i n u m r e s i s t a n c e t h e r m o m e t e r i m m e r s e d i n t h e d e c a l i n was u s e d t o m e a s u r e t h e t e m p e r a t u r e . I n t h e f i r s t s t a g e s o f t h e p u r i f i -c a t i o n an e l e c t r i c p r o p e l l e r s t i r r e r was u s e d a n d l a t e r t h i s was r e p l a c e d b y a h a n d o p e r a t e d r i n g s t i r r e r . A b o u t f i v e -s i x t h s o f t h e i s o m e r was p e r m i t t e d to f r e e z e and t h e m o t h e r l i q u o r , c o n t a i n i n g t h e i m p u r i t i e s , was p o u r e d o f f . T h i s was r e p e a t e d u n t i l a c o n s t a n t f r e e z i n g p o i n t was o b t a i n e d . T h e d e g r e e o f p u r i t y o f t h e i s o m e r was j u d g e d b y t h e l e n g t h o f t h e c o n s t a n t t e m p e r a t u r e . p e r i o d . B . D e t e r m i n a t i o n o f f r e e z i n g p o i n t s The f r e e z i n g p o i n t o f t h e p u r e i s o m e r was d e t e r m i n e d i n t h e same a p p a r a t u s b u t t h e d r y i c e was r e p l a c e d b y a n a l c o h o l b a t h t h e t e m p e r a t u r e o f w h i c h was h e l d c o n s t a n t a t t e n d e g r e e s l o w e r t h a n t h e f r e e z i n g p o i n t . S i n c e t h e p u r e i s o m e r s w e r e f o u n d t o f r e e z e c o m p l e t e l y a t a c o n s t a n t t e m -p e r a t u r e t h e r e c a n b e no d o u b t as to t h e i r p u r i t y . 9 . C. R e s u l t s T h e f i n a l r e s u l t s o b t a i n e d i n t h i s w o r k a r e shown i n t a b l e I I . T a b l e I I . I s o m e r F r e e z i n g P o i n t . 0 , n 2 0 C i s T r a n s - 4 3 . 2 5 + 0 . 2 - 3 1 . 4 9 + 0 . 2 1 . 4 8 1 1 3 1 . 4 6 9 6 8 T h e s e i s o m e r s w e r e u s e d i n t h e c a l o r i m e t r i o w o r k . 1 0 . P a r t I I . The H e a t s o f C o m b u s t i o n o f t h e I s o m e r s o f D e o a h y d r o n a p h t h a l e r i e . A p p a r a t u s A . R e a s o n s f o r c h o i c e Two means a r e a v a i l a b l e b y w h i c h t h e c o m b u s t i o n may b e b r o u g h t a b o u t i n t h e bomb i n c a l o r i m e t r i c m e a s u r e m e n t s . The o x i d a t i o n may be c a u s e d b y a n o x i d i z i n g a g e n t s u c h as NagOg o r by p u r e o x y g e n u n d e r p r e s s u r e . B e c a u s e o f t h e l a r g e number o f more o r l e s s u n c e r t a i n c o r r e c t i o n s i n v o l v e d i n t h e f o r m e r m e t h o d i t i s n e v e r u s e d f o r p r e c i s e w o r k . F o r t h i s i n v e s t i g a t i o n we c h o s e an o x y g e n bomb c a l o r i m e t e r , m a n u f a c -t u r e d b y t h e E m e r s o n A p p a r a t u s Company. T h e r e a r e two e n t i r e l y d i f f e r e n t m e t h o d s u s e d f o r bomb c a l o r i m e t r y . T h e r e i s t h e a d i a b a t i c m e t h o d d e v e l o p e d by T . W. R i c h a r d s a t H a r v a r d a n d t h e c o n s t a n t J a c k e t m e t h o d . I n t h e f o r m e r t h e t e m p e r a t u r e o f t h e j a c k e t may be k e p t t h e same a s t h a t o f t h e c a l o r i m e t e r a n d o n l y t h e i n i t i a l and f i n a l t e m p e r a t u r e s o b s e r v e d . A f t e r a c a r e f u l s t u d y o f t h e s o u r c e s o f e r r o r s a s o u t l i n e d by W h i t e ^ 2 ) a n d by D i c k i n s o n ^ 4 ) , i t was d e c i d e d t h a t t h e a d i a b a t i c m e t h o d was n o t w e l l s u i t e d to t h e (3) W h i t e , W. P . , The M o d e r n C a l o r i m e t e r . ( 4 ) D i c k i n s o n , B u l l e t i n o f t h e B u r e a u o f S t a n d a r d s , V o l . 1 1 , 1 9 1 5 . •11. p r e s e n t t y p e o f w o r k . I n t h e f i r s t p l a c e i t w o u l d h a v e b e e n a l m o s t i m p o s s i b l e to r a i s e t h e t e m p e r a t u r e o f t h e j a c k e t a s r a p i d l y a s t h e c a l o r i m e t e r t e m p e r a t u r e r o s e , and s e c o n d l y , a s p o i n t e d o u t by D i c k i n s o n , ^ ) t h e a d i a b a t i c m e t h o d o n l y r e d u c e s t h e c o r r e c t i o n s i n v o l v e d due t o c o n d u c t i o n , c o n v e c t i o n and r a d i a t i o n b e c a u s e o f t e m p e r a t u r e l a g s w h i c h o c c u r . A s a r e s u i t o f t h e s e c o n s i d e r a t i o n s i t was d e c i d e d t o u s e t h e c o n s t a n t j a c k e t t e m p e r a t u r e m e t h o d . B . A p p l i c a t i o n o f s t a n d a r d bomb o a l o r i m e t e r The c a l o r i m e t e r , a s s u p p l i e d , was t h e s t a n d a r d E m e r s o n A d i a b a t i c Bomb C a l o r i m e t e r and r e q u i r e d a number o f a l t e r a t i o n s t o make i t s u i t a b l e f o r t h i s w o r k . To k e e p t h e j a c k e t t e m -p e r a t u r e c o n s t a n t a t 2 5 ° C . i t was f o u n d n e c e s s a r y t o i n s t a l l a t h e r m o s t a t i c c o n t r o l . The t h e r m o s t a t i t s e l f was b u i l t i n t h e l a b o r a t o r y . The c o n t r o l was b r o u g h t a b o u t by t h e t h e r m a l e x p a n s i o n o f a l a r g e q u a n t i t y o f m e r c u r y i n t o a c a p i l l a r y t u b e . The t h e r m o s t a t was i m m e r s e d i n t h e j a c k e t w a t e r . A C e n c o " S u p e r s e n s i t i v e D r y C e l l R e l a y " was u s e d w i t h t h i s t h e r m o s t a t . A l t e r n a t i n g c u r r e n t was u s e d to h e a t t h e j a c k e t w a t e r , t h e w a t e r i t s e l f a c t i n g a s t h e r e s i s t o r . T h e r e was no n e e d f o r any c o o l i n g d e v i c e s i n c e t h e room t e m p e r a t u r e was a l s o m a i n t a i n e d a t 2 5 ° C . and t h e i n t e r i o r o f t h e o a l o r i m e t e r , t o w h i c h h e a t was l o s t f r o m t h e j a c k e t , was a l w a y s b e l o w j a c k e t t e m p e r a t u r e . (5) l o c . c i t . 1 2 . S i n c e t h e t o p o f t h e c a l o r i m e t e r was n o t s u r r o u n d e d b y t h e j a c k e t w a t e r i t was d e c i d e d t o m a i n t a i n t h e r o o m o t e m p e r a t u r e c o n s t a n t a t 25 0 . a n d i n t h i s way t o make t h e c a l o r i m e t e r s u r r o u n d i n g s o f c o n s t a n t t e m p e r a t u r e , T h e room c h o s e n f o r t h i s w o r k was w e l l s u i t e d f o r a c o n s t a n t t e m p e r a -t u r e , s i n c e t h e r e w e r e no windows to c a u s e d r a f t s and t h e v e n t i l a t i n g s y s t e m c o u l d be r e a d i l y o u t o f f . To m a i n t a i n t h e r o o m t e m p e r a t u r e a t 2 5 ° C . a n e l e c t r i c h e a t e r was c o n s t r u c t e d f r o m n i c h r o m e w i r e . The w i r i n g o f t h i s h e a t e r was made so t h a t b y means o f p a r a l l e l a n d s e r i e s a r r a n g e m e n t s p o w e r s u p p l i e s f r o m 240 t o 1300 w a t t s w e r e a v a i l a b l e . The a i r o f t h e r o o m was c i r c u l a t e d o v e r t h e c o i l s o f t h e h e a t e r . No t h e r m o - r e g u l a t o r was n e c e s s a r y , s i n c e i t was f o u n d t h a t , o n c e t h e r o o m h a d b e e n b r o u g h t u p t o t e m p e r a t u r e , 1000 w a t t s s u p p l i e d t o t h i s h e a t e r w o u l d m a i n t a i n r o o m t e m p e r a t u r e a t 2 5 ° C . f o r h o u r s a t a t i m e . Now t h e i d e a l c o n s t a n t j a c k e t c a l o r i m e t e r i s one i n w h i c h t h e c a l o r i m e t e r i t s e l f i s s u r r o u n d e d . b y t h e c o n s t a n t t e m p e r a t u r e j a c k e t on a l l s i d e s , b o t t o m and t o p . However i f a w a t e r - f i l l e d c o v e r i s u s e d t h e d i f f i c u l t i e s o f m a n i p u l a t i o n a r e i n c r e a s e d m a n i f o l d , a n d , i n a d d i t i o n , t h e r e a r e many s o u r c e s o f unknown e r r o r s i n t r o d u c e d . F o r e x a m p l e w a t e r may l e a k f r o m t h e c o v e r i n t o t h e c a l o r i m e t e r t h r o u g h a n y one o f t h e p a c k i n g g l a n d s u s e d f o r the s t i r r e r s h a f t , t h e r m o m e t e r (6 ) s t e m , and f i r i n g l e a d s . F o l l o w i n g t h e s u g g e s t i o n o f W h i t e ( 6 ) l o o . c i t . 1 3 . a c o p p e r c o v e r was i n s t a l l e d i n t h e s t a n d a r d c o v e r o f t h e c a l o r i m e t e r . T h i s c o v e r c o n s i s t e d o f a s h e e t o f #16 g a u g e c o p p e r w h i c h was s o l d e r e d to t h e o r d i n a r y c o v e r so t h a t , when i n p l a c e , t h e c o p p e r was i n g o o d t h e r m a l c o n t a c t w i t h t h e w a l l s o f t h e c o n s t a n t t e m p e r a t u r e j a c k e t . T h i s a d d i t i o n a l o n g w i t h t h e c o n s t a n t t e m p e r a t u r e r o o m was f o u n d t o g i v e v e r y s a t i s f a c t o r y r e s u l t s . The a p p a r a t u s a s s u p p l i e d was e q u i p p e d w i t h a n o n -c o n d u c t i n g s u p p o r t f o r t h e c a l o r i m e t e r c a n . T h e p r e s e n c e o f s u c h a n o n - c o n d u c t i n g m a t e r i a l i n t e r p o s e d b e t w e e n t h e c a l o r i -m e t e r and i t s j a c k e t I n t r o d u c e s a l a r g e e r r o r i n t h e c o n s t a n c y o f t h e c o e f f i c i e n t o f c o n d u c t i o n . By a r a t h e r l o n g m a t h e -m a t i c a l t r e a t m e n t , i t may b e shown t h a t , s i n c e t h e c o n d u c t i v i t y o f s u c h a m a t e r i a l i s s m a l l , i t c a u s e s l a r g e i r r e g u l a r i t i e s i n t h e h e a t t r a n s f e r when t h e t e m p e r a t u r e o f one s u r f a c e v a r i e s o v e r a r e l a t i v e l y w i d e r a n g e . H e n c e i t may b e s e e n t h a t a l l n o n - c o n d u c t i n g s u p p o r t s s h o u l d be n e g l i g i b l y s m a l l w i t h t h e s m a l l e s t p o s s i b l e a r e a i n c o n t a c t w i t h t h e c a l o r i m e t e r . The n o n - c o n d u c t i n g s u p p o r t was r e p l a c e d by t h r e e b r a s s c o n e s 9 mm. h i g h . E a c h cone h a d a b a k e l i t e t i p 1 . 5 mm. i n d i a m e t e r and 0 . 5 mm. h i g h . So a s t o make v e r y g o o d t h e r m a l c o n t a c t w i t h t h e j a c k e t , t h e c o n e s were s o l d e r e d t o t h e b o t t o m o f t h e j a c k e t . W i t h t h e a b o v e m e n t i o n e d a l t e r a t i o n s t o t h e c a l o r i m e t e r we o b t a i n e d t h e maximum a c c u r a c y f r o m o u r e q u i p m e n t . T h e m e a s u r e m e n t o f t h e t e m p e r a t u r e s o f t h e j a c k e t and r o o m was made w i t h m e r c u r y t h e r m o m e t e r s g r a d u a t e d t o o n e -1 4 . t e n t h o f a d e g r e e . E a c h o f t h e s e was s t a n d a r d i z e d a g a i n s t a p l a t i n u m r e s i s t a n c e t h e r m o m e t e r w h i c h i n t u r n h a d b e e n s t a n -d a r d i z e d a t t h e B u r e a u o f S t a n d a r d s . To m e a s u r e t h e t e m p e r a -t u r e r i s e o f t h e c a l o r i m e t e r a c a l o r i m e t r i c p l a t i n u m r e s i s -t a n c e t h e r m o m e t e r was u s e d . T h i s t h e r m o m e t e r , s u p p l i e d by t h e L e e d s and N o r t h r u p Company, was s i m i l a r t o t h e r e s i s t a n c e ( 7 ) t h e r m o m e t e r d e v e l o p e d by D i c k i n s o n ' a t t h e U . S . B u r e a u o f S t a n d a r d s and was o f t h e f o u r l e a d t y p e . So a s t o h a v e a min imum l a g t h e t h e r m o m e t e r h a d a s i l v e r s h e a t h . The r e s i s -t a n c e o f t h e p l a t i n u m c o i l s was m e a s u r e d by a L e e d s a n d N o r t h r u p r e s i s t a n c e b o x a n d a s e n s i t i v e b a l l i s t i c g a l v a n o m e t e r . W i t h t h i s c o m b i n a t i o n we w e r e a b l e to r e a d t h e t e m p e r a t u r e i n t e r v a l t o 0 . 8 p e r m i l l e . G . M e t h o d o f s t a n d a r d i z i n g e q u i p m e n t F o r o u r w o r k two m e t h o d s o f d e t e r m i n i n g t h e h e a t c a p a c i t y o f t h e c a l o r i m e t e r p r e s e n t e d t h e m s e l v e s . B o t h o o n s i s t o f p r o d u c i n g a known amount o f h e a t w i t h i n t h e c a l o -r i m e t e r and o b s e r v i n g t h e r i s e i n t e m p e r a t u r e . A n e l e c t r i c r e s i s t a n c e c o i l c o u l d be i m m e r s e d i n t h e c a l o r i m e t e r w a t e r and a known q u a n t i t y o f power d i s s i p a t e d i n t h e c o i l . The s e c o n d m e t h o d c o n s i s t s o f b u m i n g i n t h e bomb a m a t e r i a l whose h e a t o f c o m b u s t i o n i s a c c u r a t e l y k n o w n . The f o r m e r i s a more f u n d a m e n t a l p r o c e d u r e b u t i t h a s two d i s a d v a n t a g e s . I n t h e (V) I b i d . , V o l . 9 , 1 9 1 3 , p . 4 3 . D i c k i n s o n . 1 5 , f i r s t p l a c e , s i n c e t h e h e a t i s n o t p r o d u c e d i n t h e bomb, a f a r d i f f e r e n t h e a t i n g c u r v e r e s u l t s a n d s e c o n d l y s u c h a m e t h o d i n v o l v e s a v e r y e l a b o r a t e s e t - u p . The l a t t e r m e t h o d g i v e s a h e a t i n g c u r v e w h i c h i s i d e n t i c a l i n n a t u r e to t h a t o f t h e e x p e r i m e n t a l r u n s . Two s u b s t a n c e s w e r e c h o s e n as s t a n d a r d c a l o r i m e t r i c f u e l s . T h e s e w e r e n a p h t h a l e n e , S t a n d a r d C a l o r i m e t r i c S a m p l e N o . 3 8 b , and b e n z o i c a c i d , S t a n d a r d C a l o r i m e t r i c S a m p l e N o . 3 9 e . B o t h t h e s e w e r e s u p p l i e d by t h e N a t i o n a l B u r e a u o f S t a n d a r d s a t W a s h i n g t o n . I t was f o u n d t h a t w i t h o u r e q u i p m e n t we c o u l d n o t g e t c o m p l e t e c o m b u s t i o n w i t h t h e b e n z o i c a c i d , b u t t h e n a p h t h a l e n e g a v e no s u c h t r o u b l e . When a c h a r g e was b u r n e d i n t h e bomb, h e a t was p r o d u c e d f r o m t h r e e s o u r c e s , i n a d d i t i o n t o t h a t p r o d u c e d by t h e c o m b u s t i o n o f t h e c h a r g e i t s e l f . H e a t was p r o d u c e d by t h e p a s s a g e o f t h e f i r i n g c u r r e n t t h r o u g h t h e f u s e w i r e , b y t h e c o m b u s t i o n o f t h e w i r e i t s e l f , and b y t h e p r o d u c t i o n o f n i t r i c a c i d f r o m t h e n i t r o g e n p r e s e n t i n t h e bomb. T h e s e t h r e e e r r o r s w e r e a l s o p r e s e n t when t h e e x p e r i m e n t a l r u n s w e r e made; h e n c e , when o n c e d e t e r m i n e d , t h e y c o u l d b e u s e d t h r o u g h o u t a l l c a l -c u l a t i o n s . To d e t e r m i n e t h e h e a t g i v e n o u t b y t h e p a s s a g e o f t h e f i r i n g c u r r e n t and by t h e c o m b u s t i o n o f t h e i r o n w i r e t h e bomb was a s s e m b l e d i n t h e u s u a l way and i m m e r s e d i n t h e c a l o -r i m e t e r w a t e r , w h i c h was p r e v i o u s l y h e a t e d t o 2 5 ° C . , i . e . t o t h e j a c k e t t e m p e r a t u r e . When c o n d i t i o n s were s t e a d y t h e w i r e was f i r e d and t h e i n c r e a s e i n r e s i s t a n c e o f t h e t h e r m o m e t e r n o t e d . T h i s i n c r e a s e was n o t c o n v e r t e d t o a t e m p e r a t u r e r i s e 1 6 . s i n c e i t c o u l d be u s e d d i r e c t l y i n t h e c a l c u l a t i o n s , The h e a t p r o d u c e d b y t h e f o r m a t i o n o f n i t r i c a c i d i n t h e bomb was c a l c u l a t e d f r o m t h e q u a n t i t y o f a c i d f o r m e d . A f t e r a r u n t h e i n t e r i o r o f t h e bomb was c a r e f u l l y w a s h e d o u t w i t h d i s t i l l e d w a t e r a n d t h e w a s h w a t e r c o l l e c t e d . The c a r b o n d i o x i d e was r e m o v e d b y b o i l i n g t h e s o l u t i o n a n d t h e n i t r i c a c i d p r e s e n t t i t r a t e d w i t h s t a n d a r d s o d i u m h y d r o x i d e w i t h p h e n o l p h t h a l e i n a s an i n d i c a t o r . T h e c o r r e c t i o n f o r t h e f o r m a t i o n o f a q u e o u s n i t r i c a c i d i s 62 k i l o j o u l e s p e r m o l e , o r 0 , 9 8 k i l o j o u l e s p e r g r a m o f n i t r i c a c i d . F r o m t h e m e a s u r e d r i s e i n t e m p e r a t u r e , p r o d u c e d i n t h e s t a n d a r d i z i n g r u n s a n d t h e known q u a n t i t y o f h e a t p r o d u c e d , w i t h t h e c o r r e c t i o n s o u t l i n e d a b o v e , t h e h e a t c a p a c i t y o f t h e , c a l o r i m e t e r was d e t e r m i n e d . E x p e r i m e n t a l P r o c e d u r e The p r o c e d u r e f o l l o w e d i n t h e r u n s o n n a p h t h a l e n e a n d b e n z o i c a c i d and i n t h e r u n s on t h e d e c a h y d r o n a p h t h a l e n e s a m p l e s was t h e same. A t t h e s t a r t o f e a c h r u n t h e t h r e a d s o f t h e bomb w e r e c a r e f u l l y c l e a n e d o u t w i t h b e n z e n e a n d g r e a s e d w i t h a g o o d l u b r i c a n t . One c u b i c c e n t i m e t e r . o f w a t e r was p i p e t t e d i n t o t h e bomb t o s a t u r a t e t h e a i r b e f o r e t h e r u n , a n d 3 . 2 5 i n c h e s o f #36 B&S g a u g e i r o n w i r e a t t a c h e d t o t h e two t e r m i n a l s i n t h e bomb. The s a m p l e was w e i g h e d o u t i n t o t h e n i c k e l c o m b u s t i o n p a n and t h e l a t t e r i m m e d i a t e l y p l a c e d i n i t s s u p p o r t i n t h e bomb and t h e bomb c o v e r p u t o n . I n t h e c a s e 1 7 . o f n a p h t h a l e n e a n d b e n z o i c a c i d t h e p a n was f i r s t w e i g h e d , a b o u t 0 . 9 g r a m s o f c o m b u s t i b l e p l a c e d i n i t a n d c a r e f u l l y f u s e d , so t h a t on c o m b u s t i o n t h e r e was no s p a t t e r i n g . A f t e r c o o l i n g , t h e p a n and i t s c o n t e n t s w e r e a g a i n w e i g h e d , a n d f r o m t h e d i f f e r e n c e , t h e w e i g h t o f t h e c o m b u s t i b l e d e t e r m i n e d . When t h e bomb h a d b e e n s e a l e d i t was f i l l e d w i t h o x y g e n t o a p r e s s u r e o f 30 a t m o s p h e r e s a t 2 5 ° 0 . T h e o u t s i d e o f t h e bomb was c a r e f u l l y c l e a n e d w i t h b e n z e n e a n d , a f t e r t h e f i r i n g l e a d s h a d b e e n a t t a c h e d , i t was p l a c e d i n t h e c a l o r i m e t e r c a n . The d i s t i l l e d w a t e r t o be u s e d i n t h e c a l o r i m e t e r was f r e e d o f a i r and c o o l e d t o a b o u t 1 8 ° C . so t h a t a t a l l t i m e s d u r i n g t h e r u n t h e t e m p e r a t u r e o f t h e c a l o r i m e t e r w o u l d be b e l o w t h a t o f t h e j a c k e t . Two t h o u s a n d e i g h t y g r a m s o f t h i s w a t e r w e r e t h e n w e i g h e d out w i t h i n an a c c u r a c y o f 0 . 0 5 gm. The a p p a r a t u s was t h e n a s s e m b l e d and t h e f o r e - r a t i n g p e r i o d h e a t i n g r a t e d e t e r m i n e d . T h i s p e r i o d was a b o u t t w e n t y m i n u t e s i n l e n g t h and d u r i n g i t t h e r e s i s t a n c e o f t h e t h e r m o m e t e r was m e a s u r e d a t m i n u t e i n t e r v a l s . The c h a r g e was t h e n f i r e d a n d t h e t i m e d e t e r m i n e d when t h e r e s i s t a n c e h a d gone u p i n s t e p s o f 0 . 0 3 o h m s . The r a t e o f r e s i s t a n c e r i s e i n t h e a f t e r r a t i n g p e r i o d was d e t e r m i n e d a s i n t h e f o r e - r a t i n g p e r i o d . The r u n was t h e n c o m p l e t e and t h e a p p a r a t u s d i s m a n t l e d . C a l c u l a t i o n s . A . M e t h o d u s e d t o c a l c u l a t e c o o l i n g c o r r e c t i o n T h e r e a r e a n u m b e r o f m e t h o d s w h i c h h a v e b e e n u s e d 1 8 . t o c a l c u l a t e t h e c o o l i n g c o r r e c t i o n o r i n o u r c a s e t h e h e a t i n g ( 8 ) c o r r e c t i o n . I t was d e c i d e d t o u s e t h a t g i v e n by D i o k i n s o n • He shows t h a t no a p p r e c i a b l e e r r o r i s i n t r o d u c e d i f t m , t h e t i m e a t w h i c h t h e two a r e a s u n d e r t h e h e a t i n g c u r v e a r e e q u a l , i s t a k e n as t h e t i m e f o r 0 . 6 o f t h e r i s e t o t a k e p l a c e . The h e a t g a i n e d f r o m t h e s u r r o u n d i n g s f r o m t h e t i m e o f f i r i n g t o t i s e q u a l t o t m t i m e s t h e h e a t i n g r a t e i n t h e f o r e - r a t i n g p e r i o d . The h e a t g a i n e d f r o m t h e s u r r o u n d i n g s a f t e r t i s e q u a l t o t h e p r o d u c t o f t h e t i m e f r o m t m t i l l a c o n s t a n t h e a t i n g r a t e i s o b t a i n e d t i m e s t h i s h e a t i n g r a t e . The sum o f t h e s e two h e a t s i s e q u a l t o t h e t o t a l h e a t g a i n e d f r o m t h e s u r r o u n d i n g s d u r i n g t h e x - p e r i o d . ( 8 ) I b i d . , V o l . 1 1 , 1 9 1 5 , p . 229 e t s e q . D i c k i n s o n . 1 9 . B . R e s u l t s : H e a t C a p a c i t y o f Bomb Run Mo „ W t . o f N a p h -t h a l e n e W t . o f W a t e r C o r r e c t e d R e s i s t a n c e Temp. R i s e H e a t C a p a c i t y K i l o j o u l e s B e f o r e A f t e r 9 . 8 2 9 3 • •• 2 0 8 0 . 4 • 2 7 . 5 3 8 5 2 7 . 8 5 4 2 3 i 1 3 5 0 1 0 . 6 5 4 4 10 . 7 5 1 6 2 0 8 0 . 5 2 7 . 4 6 2 6 2 7 . 7 4 8 6 2 i 8 3 9 4 1 0 . 6 6 3 2 11 . 7 8 0 3 2 0 8 0 . 5 2 7 . 8 1 9 5 2 8 . 1 1 6 1 2 . 9 4 7 6 1 0 . 6 6 3 0 • H e a t C a p a c i t y o f bomb p l u s 2080 g m s . o f w a t e r = 1 0 . 6 6 0 2 k i l o j o u l e s . H e a t o f C o m b u s t i o n o f C i s D e c a l i n Run 'No. W t . o f S a m p l e W t . o f W a t e r , C o r r e c t e d B e f o r e . R e s i s t a n c e A f t e r Temp. R i s e H e a t o f C o m b u s t i o n K i l o j o u l e s / g m . 14 . 7 5 2 3 2 0 8 0 . 2 2 7 . 8 6 1 0 2 8 . 1 8 4 2 3 i 2 1 2 6 4 5 * 4 5 0 16 2 0 8 0 . 1 2 7 . 2 0 4 8 2 7 . 5 2 4 5 3 . 1 7 1 7 4 5 . 6 5 9 17 . 7 5 7 6 2 0 8 0 . 3 27*1032 2 7 . 4 2 8 4 3 . 2 2 5 4 4 5 . 3 1 5 H e a t o f c o m b u s t i o n o f G i s . d e c a l i n 4 5 . 4 7 5 k i l o j o u l e s / g m . H e a t o f C o m b u s t i o n o f T r a n s D e c a l i n Run W t . o f W t . o f C o r r e c t e d R e s i s t a n c e Temp. Heat o f N o . S a m p l e W a t e r B e f o r e A f t e r R i s e C o m b u s t i o n L L l o j o u l e s / g m . 19 . 7 5 1 6 2 0 8 0 . 2 2 7 . 4 7 8 0 2 7 . 8 0 0 4 3 . 2 0 1 0 4 5 . 3 3 0 20 . 7 6 6 8 2 0 8 0 . 4 2 7 . 7 2 8 5 2 8 . 0 5 6 5 3 . 2 5 9 0 4 5 . 2 4 1 21 . 7 3 7 8 2 0 8 0 . 6 2 7 . 2 5 1 7 2 7 . 5 6 7 9 3 . 1 3 8 4 4 5 . 2 8 0 22 . 7 6 8 2 2 0 8 0 . 3 . 2 7 . 1 5 3 8 2 7 . 4 8 3 1 3 . 2 6 6 5 4 5 . 2 6 0 H e a t o f C o m b u s t i o n o f T r a n s d e c a l i n = 4 5 . 2 7 8 k i l o j o u l e s / g m . 20, 2 7 . 5 3 7 1 ohms 2 7 . 8 6 0 2 " . 3 2 3 1 " 0 . G a l o u l a t i o n o f h e a t o a p a o i t y o f bomb Run N o . 9 . R e s i s t a n c e a t t i m e o f f i r i n g R e s i s t a n c e 8 m i n . a f t e r f i r i n g I n c r e a s e i n r e s i s t a n c e 0 . 6 o f R i s e = . 1 9 3 9 T ime f r o m f i r i n g t m = 4 8 . 5 " -F o r e - h e a t i n g r a t e . 0 0 1 7 o h m s / m i n F o r e c o r r e c t i o n j i ^ j f . 0 0 1 7 ) = . 0 0 1 4 A f t e r - h e a t i n g r a t e 0 . 0 0 0 8 ohms/min A f t e r c o r r e c t i o n ( 4 8 0 - 4 8 . 5 ) Q 0 Q 8 a , 0 0 5 7 ( 6 0 ) R i s e c o r r e c t e d f o r e x t e r n a l h e a t i n g . 3 2 3 1 - . 0 0 7 1 « . 3 1 6 0 R i s e due t o c o m b u s t i o n o f i r o n w i r e = . 0 0 0 3 C o r r e c t e d r i s e 0 . 3 1 5 7 o h m s . F o r e R e s i s t a n c e = 2 7 . 5 3 7 1 + . 0 0 1 4 = 2 7 . 5 3 8 5 A f t e r R e s i s t a n c e .« 2 7 . 5 3 8 5 + . 3 1 5 7 = 2 7 . 8 5 4 2 R i s e i n t e m p e r a t u r e c a l c u l a t e d f r o m C a l l e n d a r f o r m u l a = 3 . 1 3 5 0 W e i g h t o f N a p h t h a l e n e = 0 . 8 2 9 3 H e a t g i v e n o u t by n a p h t h a l e n e = ( 4 0 . 2 1 5 ) ( . 8 2 9 3 ) = 3 3 . 3 5 1 k i l o j o u l e s H e a t t o r a i s e 0 . 4 gm. w a t e r = ( 0 . 4 ) ( 3 . 1 4 ) ( . 0 0 4 1 8 3 ) = . 0 0 5 H e a t g i v e n o u t b y f o r m a t i o n o f HN0 r = . 0 5 7 H e n c e n e t h e a t « 3 3 . 4 0 2 H e a t c a p a c i t y o f A p p a r a t u s = 1 0 . 6 5 4 4 k i l o j o u l e s . 8 1 . D. C a l c u l a t i o n o f h e a t o f c o m b u s t i o n Run N o . 1 4 . The m e t h o d e m p l o y e d t o c a l c u l a t e c o r r e c t e d t e m p e r a t u r e r i s e was t h e same a s g i v e n f o r Run # 9 . C o r r e c t e d t e m p e r a t u r e r i s e 3 . 2 1 8 6 H e a t a b s o r b e d b y bomb ( I G . 6 6 0 2 ) ( 3 . 2 1 2 6 ) = 3 4 . 2 4 6 H e a t a b s o r b e d b y 0 , 2 g m s . w a t e r ( . 2 ) ( 3 . 2 1 ) ( , 0 0 4 1 8 3 ) = , 0 0 3 H e a t g i v e n o u t by p r o d u c t i o n o f HN0_ - . 0 5 7 3 H e n c e n e t h e a t o u t 3 4 . 2 4 6 + . 0 0 3 - . 0 5 7 = 3 4 . 1 9 2 W e i g h t o f C i s d e c a l i n w e i g h e d i n v a c u o . 7 5 1 4 + ( . 7 5 ) ( . 0 0 1 1 9 ) = . 7 5 2 3 H e a t o f c o m b u s t i o n o f C i s d e c a l i n = ^ T B i n F = 4 5 . 4 5 0 k i l o j o u l e s / g m . D i s c u s s i o n o f R e s u l t s . The r e s u l t s o f t h i s i n v e s t i g a t i o n show t h e h e a t s o f c o m b u s t i o n o f t h e i s o m e r s o f d e c a h y d r o n a p h t h a l e n e t o b e : C i s i s o m e r - 4 5 . 4 7 5 ± . 0 3 3 k i l o j o u l e s a t 2 5 ° C . T r a n s , i s o m e r - 4 5 . 2 7 8 ± . 0 3 3 k i l o j o u l e s a t 2 5 ° 0 . To c o m p a r e t h e s e w i t h o t h e r p u b l i s h e d r e s u I t s c o n v e r t t h e s e v a l u e s t o 1 5 ° c a l o r i e s . C i s i s o m e r - 1 0 , 8 7 1 ± 8 o a l . T r a n s i s o m e r - 1 0 , 8 2 4 + 8 c a l . . 2 2 . • • H u o k e l ^ ^ Ogives v a l u e s f o r t h e two i s o m e r s T r a n s f r o m o o t a l i n 1 0 , 8 2 4 + 5 o a l . T r a n s f r o m teehn. 1 0 , 8 4 4 ± 11 o a l . T r a n s a c c o r d i n g t o G lemmensen 1 0 , 8 2 7 + 1 c a l . G i s f r o m o o t a l i n 1 0 , 8 5 2 ± 6 o a l . G i s f r o m t e c h n . 1 0 , 8 6 5 ± 16 c a l . R o t h and L a s s e ^ 1 0 r e p o r t 1 0 , 8 5 6 ± 8 c a l . f o r t r a n s d e c a l i n and 1 0 , 8 5 8 + 7 c a l . f o r c i s d e c a l i n . F r o m t h e s e v a l u e s i t may b e seen t h a t o u r r e s u l t s agree very w e l l with t h o s e r e p o r t e d by o t h e r i n v e s t i g a t o r s . ( 9 ) H u c k e l , A n n . 4 4 1 , 1, 1 9 2 5 . ( 1 0 ) R o t h and L a s s e , A n n . 4 4 1 , 5 2 , . 1 9 2 5 . 23o Bibliography. Dickinson, H. C., B u l l e t i n of the Bureau of Standards, Vol 9, 1913, Vol 11, 1915. Huckel, W., Annalen der Chemie, 44-1, 1, 1925. Roth, W. and Lasse, R., Annalen der Chemie, 441 f 52, 1925* Walker, R. Do, M.A.Sc. Thesis 1937. White, V.r. P», The Modern Calorimeter. 

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