S t a n f o r d Geothermal Program I n t e r d i s c i p l i n a r y Research i n Engineering and E a r t h S c i e n c e s Stanford University Stanford, California c THE EFFECTS OF TEMPERATURE AND PRESSURE ON ABSOLUTE PERMEABILITY OF SANDSTONES c by Muhammadu Aruna April 1976 T h i s r e s e a r c h was c a r r i e d o u t under Research Grant GI- 34925 by t h e N a t i o n a l Science Foundation - ACKNOWLEDGEMENT I T h e a u t h o r would l i k e t o e x p r e s s h i s s i n c e r e a p p r e c i - I a t i o n t o h i s a d v i s e r , D r . Henry J. Ramey, Jr., for h i s i n s t r u c t i o n and g u i d a n c e t h r o u g h o u t t h e r e s e a r c h work. He I made it p o s s i b l e f o r t h e a u t h o r t o come t o S t a n f o r d U n i v e r s i l y I and c o m p l e t e h i s g r a d u a t e s t u d i e s s u c c e s s f u l l y . I I I I The a s s i s t a n c e and p r a c t i c a l s u g g e s t i o n s from t h e I I f a c u l t y o f t h e Department o f P e t r o l e u m E n g i n e e r i n g , p a r t i c u I l a r l y from Dr. W. E . Brigham and D r . a r e g r a t e f u l l y acknowledged. S u l l i v a n S . Marsden, 1 The c o o p e r a t i o n I e n j o y e d from t h e d e p a r t m e n t s e c r e t a r i e s , e s p e c i a l l y from A l i c e Mansouria4, I w i l l not be forgotten. I Many t h a n k s a r e due t o m y f r i e n d s , p a r t i c u l a r l y R o r i o A r i h a r a , H. K . Chen, and P a u l A t k i n s o n , f o r t h e i r h e l p f u l ~ I comments and Timely h e l p t h r o u g h the d a y s of e x p e r i m e n t a l w&k. C r e d i t f o r m d i f i c a t i o n of t h e a p p a r a t u s b u i l t by Wei4 b r a a d t and Cass6 i s due Jon Grim, t h e P e t r o l e u m E n g i n e e r i n g 1 Dezs-tnent m a c h i n i s t . F i n a l l y , Dr. F. Ca.ss6 reviewed t h i s m a n u s c r i p t and ma& E?--: ? s l p f u l I sugg3stions'. ~ ?>lis w s ~ kwas fund.ed u n d e r N a t i o n a l S c i e n c e Foundatiovl pm= _-'7.3L..-r- GI- 34925. I i T h i s r e p o r t was p r e p a r e d o r i g i n a l l y as a d i s s e r t a t i o n sub,mitted to t h e Department of Petroleum E n g i n e e r i n g and t h e Committee on t h e Graduate D i v i s i o n of S t a n f o r d U n i v e r s i t y i n p a r t i a l f u l f i l l m e n t of the requirements f o r the d e g r e e of Doctor of Philosophy. ii DEDICLTED TO MY PARENTS AND ALL THE GOOD PEOPLE I N MY L I F E I iii J J J J J ABSTUCT The s t a n d a r d procedurle f o r d e t e r m i n i n g t h e p e r m e a b i l i t y c of porous media a c c o r d i n g t:o API Code Mo. 2 7 i s b a s e d on t h e fundamental a s s u m p t i o n t h a t : , as l o n g as v i s c o u s f l o w p r e v a i l s , I I ' t h e a b s o l u t e p e r m e a b i l i t y of a porous medium i s a p r o p e r t y of t h e medium, a n d i s independlent of t h e f l u i d u s e d i n i t s deter-11 m i n a t i o n , s l i p e f f e c t b e i n g t a k e n i n t o a c c o u n t i n t h e case of gas f l o w . Absolute permeability has, t h e r e f o r e , been t r a d i t i o d - a l l y measured a t room c o n d i t i o n s , w i t h t h e a s s u m p t i o n t h a t it I changes o n l y w i t h o v e r b u r d e n p r e s s u r e and n o t w i t h t e m p e r a t u r e + R e s u l t s o b t a i n e d a t room t e m p e r a t u r e may t h e n b e u s e d t o p r e d i c t performance a t r e s e r v o i r c o n d i t i o n s a f t e r c o r r e c t i o n f o r I 1 ~ r e d u c t i o n by s t r e s s e f f e c t s . 11 Although t h i s a s s u m p t i o n i s t r u e for m o s t f l u i d s , r e s u l t s of r e c e n t a b s o l u t e p e r m e a b i l i t y measurements of water flow t h r o u g h p o r o u s media a t h i g h t e m p e r a t u r e s I I I and h i g h o v e r b u r d e n p r e s s u r e s d i f f e r from room c o n d i t i o n v a l u e s . Not o n l y was t h e a b s o l u t e p e r m e a b i l i t y t o water a t h i g h c o n f i n i n g p r e s s u r e l o w e r t h a n t h a t to1 o t h e r f l u i d s u s e d a t room t e m p e r a - t u r e , b u t also, t h e r e was a s i g n i f i c a n t p e r m e a b i l i t y r e d u c t i o n ~l a t elevated temperatures. An e x i s t i n g p e r m e a n e t e r w a s m o d i f i e d t o e n a b l e f l o w o f I d i f f e r e n t f l u i d s t h r o u g h s e p a r a t e flow l i n e s . Distilled water, a w h i t e m i n e r a l o i l , n i t r o p e n and 2 - o c t a n o l were t h e iv I f l u i d s u s e d , and t e s t s were c a r r i e d o u t on n a t u r a l c o n s o l i d a t e d s a n d s t o n e s and u n c o n s o l i d a t e d s i l i c a s a n d . With t h e e x c e p t i o n of w a t e r , t h e a b s o l u t e p e r m e a b i l i t i e s of t h e cores t o o t h e r f l u i d s showed l i t t l e o r no t e m p e r a t u r e dependence. The r e d u c t i o n i n p e r m e a b i l i t y t o w a t e r w i t h 11 t e m p e r a t u r e i n c r e a s e w a s a t t r i b u t e d t o i n t e r a c t i o n between water and s i l i c a . I n t h e case of water f l o w t h r o u g h geothermd 1 s y s t e m s o r i n t h e r m a l r e c o v e r y p r o c e s s e s which c a u s e l a r g e I c h a n g e s i n f o r m a t i o n t e m p e r a t u r e s , t h e e f f e c t of t e m p e r a t u r e s l on a b s o l u t e p e r m e a b i l i t y s h o u l d be c o n s i d e r e d i n e n g i n e e r i n g calculations. I V TASLE - OF CONTENTS Page ................... ABSTRACT, . . . . . . . . . . . . . . . . . . . . . . . TABLE OF CONTENTS . . . . . . . . . . . . . . . . . . L I S T OF TABLES. . . . . . . . . . . . . . . . . . . . L I S T OF FIGURES . . . . . . . . . . . . . . . . . . . ACKNOWLEDGEMENT iv V vii X xi CFAPTERS INTRODUCTION. 1 2. FLOW 4 2.1 2.2 ...... 2 . 4 V i s c o - I n e r t i a l Flow. . . . . . . . . . LITERATURE. . . . . . . . . . . . . . . . . EXPERIMENTAL EQUIPMENT. . . . . . . . . . . 4 . 1 General D e s c r i p t i o n . . .. . . 4 . 2 C o r e Holder. . . . . . . . . . . . . . 4.3 A i r B a t h and T e m p e r a t u r e C o n t r o l . . . 4.4 L i q u i d and Gas S o u r c e s . . . . . . . . 2.3 3. 4. c ............... I N POROUS YEDIA. . . . . . . . . . . . D a r c y ' s Law. . . . . . . . . . . . . . D a r c y ' s Law for Gas Flow . . . . . . . 1. c 4.5 4.6 4.7 S l i p Phenomena i n G a s F l o w ............. Hydraulic Hand P u n y . . . . . . . . . . Heat Exchangers. . . . . . . . . . . . Liq,uid Pumps L vi 4 5 ' 6 1; 7 9 15 1 15 ~ 18 18 20 21 21 21 ' T a b l e of C o n t e n t s , c o n t i n u e d Page ..... 4.8 B a c k p r e s s u r e Valve 4.9 Flow Rate M e a s u r i n g D e v i c e s . Liquid Flow 22 4.9- 2 Gas F l o w 23 PROCEDURE 5.1 Core . 23 ............ Preparation . . . . . . 5.1- 1 5.1- 2 6. 22 4.9- 1 4 - 1 0 Pressure R e c o r d i n g D e v i c e s 5. 22 25 25 25 U n c o n s o l i d a t e d O t t a w a Sand 26 . 5.2 E s t a b l i s h i n g Run C o n d i t i o n s . 5.3 Measurements and C a l c u l a t i o n s . 6.2 6.3 6.4 6.5 27 28 5.3- 1 Liquid Flow 28 5.3- 2 Gas Flow 37 ANALYSIS OF RESULTS AND DISCUSSION. 6.1 J C o n s o l i d a t e d M a s s i l l o n Sands t o n es Water Flow ........... . 41 41 6.1- 1 Consolidated Sandstones 41 6.1- 2 U n c o n s o l i d a t e d Sand 43 ........... 48 6.2- 1 Consolidated Sandstones 50 6.2- 2 U n c o n s o l i d a t e d Sand 56 G a s Flow ......... 2-Octanol Flow . . . . . . Discussion . . . . . . . . O i l Flow 3 56 58 62 7. C ONC LU S I O N S AND R.EC OIWENDAT I O N S 65 8. REFERENCES. .......... 67 vii 3 J Table of C o n t e n t s , c o n t i n u e d 9. APPENDICES. .. .... .- ... .... ...... 9.1 L i s t of T a b u l a t e d Data 9.2 C o r e Data. 70 .. .... . 9.4 L i s t of M a n u f a c t u r e r s . . . . . . . . NOMENCLATURE. .... ..... 9.3 10. Page D e r i v a t i o n s of E q u a t i o n s , c viii 71 90 94 99 102 - 'LI'ST OF TABLES I I Table 1 Page D e n s i t y a n d V i s c o s i t y of Water v s . Temperature 72 2 Viscosity 73 3 V i s c o s i t y of Chevron . O i l No. Temperature 74 Density of 75 ................. of N i t r o g e n vs. Temperature . . . . . . . . . . . .3 .vs.. . . . . . . 2-Octanol vs. T e m p e r a t u r e . . . . . V i s c o s i t y of 2-Octanol v s . Temperature. ... 10 11 12 13 14 15 F l o w D a t a for M a s s i l l o n S a n d s t o n e Core N o . Water Flow. . . . . . . . . . . . . . . . .3 ,. 78 Flow D a t a for M a s s i l l o n S a n d s t o n e Core No. 4, Water Flow. 80 ................. Flow Data for M a s s i l l o n S a n d s t o n e Core N o . 5, N i t r o g e n Flow . . . . . . . . . . . . . . . . F l o w D a t a for M a s s i l l o n Sandstone Core N o . 6 , N i t r o g e n Flow . . . . . . . . . . . . . . . . F l o w Data for P ? a s s i l l o n S a n d s t o n e Core N o . 1 0 , O i l Flow. . . . . . . . . . . . . . . . . Flow Data for M a s s i l l o n S a n d s t o n e Core N o . 11, O i l Flow. F l o w Data f o r Sand Core N o . Flow Data f o r Sand Core No. ................ Unconsolidated O t t a w a S i l i c a 1 4 , Water Flow. . . . . . . . . Unconsolidated O t t a w a S i l i c a 1 5 , Water Flow. . . . . . . . . !I I 76 77 , 11 1 iI 81 I 82 84 I 85 I I I 86 87 F l o w Data for U n c o n s o l i d a t e d O t t a w a S i l i c a Sand Core N o . 1 6 , N i t r o g e n Flow a n d Water Flow.. 88 I! Flow Data f o r U n c o n s o l i d a t e d O t t a w a S i l i c a Sand Core No. 1 7 , 2-Octanol Flow. 89 'I ................... 16 1 F l o w D a t a f o r M a s s i l l o n S a n d s t o n e Core N o . Water Flow. . . . . . . . . . . . . . . . .2,. I I ...... ix LIST - OF FIGUP,ZS Page - Figure 4 5 D e n s i t y of Water1 v s . T e m p e r a t u r e of 2 0 0 p s i g 6 Water V i s c o s i t y v s . T e m p e r a t u r e a t 2 0 0 p s i g 7 2 3 8 9 10 11 12 c .. .. .. .. ......... D e t a i l s of Assembly i n t h e A i r B a t h . . . S c h e m a t i c Diagra.m o f A p p a r a t u s . . . . . . Schematic Diagram of t h e Core H o l d e r . . . 1 13 14 15 P h o t o g r a p h of A p p a r a t u s 16 16 17 19 31 . 32 D e n s i t y v s . T e m p e r a t u r e for Chevron White Oil No. 3 a t 14.7 p s i ......... 33 V i s c o s i t y v s . Temperature for Chevron White OilNo. 3 . . 34 D e n s i t y of 2-Octanol v s . T e m p e r a t u r e a t 1 4 . 7 psi 35 .. ...... ......... ..................... V i s c o s i t y of 2-Octanol v s . T e m p e r a t u r e . . . . V i s c o s i t y of N i t r o g e n v s . T e m p e r a t u r e . .. ~ 36 39 Water P e r m e a b i l i t y v s . T e m p e r a t u r e , M a s s i l l o n S a n d s t o n e Core No. 2 . 42 Water P e r m e a b i l i t y S a n d s t o n e Core No. 44 ........... vs. Temperature, Massillon 3. . . ......... Water P e r m e a b i l i t y v s . T e m p e r a t u r e a t a C o n s t a n t C o n f i n i n g P r e s s u r e of 3000 p s i g , M a s s i l l o n S a n d s t o n e Core No. 3 . ....... 45 Water P e r m e a b i l i t y vs. T e m p e r a t u r e , M a s s i l l o n S a n d s t o n e Core No. 4 . 46 ............ 16 Water P e r m e a b i l i t y v s . T e m p e r a t u r e , Unconsolid a t e d O t t a w a S i l i c a Sand Core N o . 1 4 . 47 17 Water P e r r r - e a h i l i t y v s . T e m p e r a t u r e , O t t a w a S i l i c a Sand Core No. 1 5 .... ......... . X 49 , J L i s t df €Figures, c o n t i n u e d Figure 18 Page Apparent P e r m e a b i l i t y vs. Xeciprocal Mean P r e s s u r e a t S e v e r a l T e m p e r a t u r e s for M a s s i l l o n Core No. 5. 51 M o d i f i e d V i s c o - I n e r t i a l Graph, M a s s i l l o n C o r e N o . 5 w i t h N i t r o g e n Flow 52 .......... 19 20 21 ........ A p p a r e n t P e r m e a b i l i t y v s . I i e c i p r o c a l Mean P r e s s u r e a t S e v e r a l T e m p e r a t u r e s for M a s s i l l o n S a n d s t o n e Core N o . 6 , C o n f i n i n g P r e s s u r e = 1000 p s i g 53 .................. P e r m e a b i l i t y v s . R e c i p r o c a l Mean Apparent P r e s s u r e a t S e v e r a l T e m p e r a t u r e s for Mass i l l o n S a n d s t o n e Core 110. 6 , C o n f i n i n g Pressure 3000 p s i g . . 22 ............... 54 J A p p a r e n t P e r m e a b i l i t y vs. R e c i p r o c a l Mean P r e s s u r e a t S e v e r a l Temperatures for M a s s i l l o n S a n d s t o n e Core No. 6 , C o n f i n i n g P r e s s u r e = 4000 p s i g 55 .................. 23 24 A p p a r e n t P e r m e a b i l i t y v s . R e c i p r o c a l Mean P r e s s u r e a t S e v e r a l T e m p e r a t u r e s for O t t a w a S i l i c a Sand Core No. 1 6 , C o n f i n i n g P r e s s u r e = 2000 p s i g .................. O i l P e r a e a b i l i t y 'vs. T e E p e r a t u r e for M a s s i l l o n Core So. 10 . . . . . . . . . . . . . . . . . J 57 59 25 O i l P s r n e a b i l i t y v s . T e m p e r a t u r e for M a s s i l l o n CcFe KO. 11 60 26 2 - O c ~ z n o l P e r m e a b i l i t y vs. ................. Temperature f o r U n c c r - s o i i d a t e d O t t a w a S i l i c a Sand Core N o . 1 7 61 J J J 1,. L?VIiODUCTION A long held conclusion t h a t t h e absolute permeability of a p o r o u s medium i s a c o n s t a n t d e t e r m i n e d o n l y by t h e s t r u c t u r e of t h e medium i n q u e s t i o n i s t h e s u b j e c t of t h i s study. Experiments d e s i g n e d t o m e a s u r e t h e a b s o l u t e p e r - m e a b i l i t y of porous media h a v e shown t h a t the absolute , ~ p e r m e a b i l i t y t o water f o r c e r t a i n s a n d s t o n e c o r e s v a r i e s w i t + t h e l e v e l of c o n f i n i n g p r e s s u r e as w e l l as w i t h t e m p e r a t u r e . F o r w a t e r f l o w , p e r m e a b i l i t y r e d u c t i o n s of up t o 6 0 % were I o b s e r v e d when t e m p e r a t u r e was i n c r e a s e d f r o m 7OoF t o 30OoF. I This i m p o r t a n t d i s c o v e r y m y h a v e s i g n i f i c a n t r a m i f i I c a t i o n s i n many o i l r e c o v e r y by thermal p r o c e s s e s . The i n - 1 1 I j e c t i o n of h o t water and steam i n t o o i l r e s e r v o i r s , underg r o u n d c o m b u s t i o n , i n j e c t i o n of f l u i d s i n t o w e l l s , t h e prod u c t i o n of g e o t h e r m a l e n e r g y , and t h e d i s p o s a l o f atomic waste p r o d u c t s i n p o r o u s f o r m a t i o n s a l l c a u s e changes i n I formation temperatures. I n r e s e r v o i r engineering, a b s o l u t e permeability i s a b a s i c p a r a m e t e r which h a s o f t e n b e e n measured a t room con- ~1 d i t i o n s , w i t h t h e i m p l i c i t assumption t h a t only confining p r e s s u r e affected the r e s u l t . (Of c o u r s e w e i g n o r e t h e w e 1 4 known r e a c t i o n s between w a t e r and c l a y s . 1 Hitherto, there- f o r e , a s i n g l e value of a b s o l u t e p e r m e a b i l i t y throughout a r a n g e of r e s e r v o i r t e m p e r a t u r e s has b e e n used in r e s e r v o i r engineering calculations. t d Weinbrandtl' found foir water f l o w , t h a t t h e a b s o l u t e p e r m e a b i l i t y of c o n f i n e d , f i r e d s a n d s t o n e cores w a s s t r o n g l y temperature dependent. 2 J Casse v e r i f i e d t h e Weinbrandt r e s u l t . I n r a i s i n g t h e t e m p e r a t u r e l e v e l of a f i r e d c o n s o l i d a t e d s a n d s t o n e core u n d e r a c o n f i n i n g p r e s s u r e of 2 0 0 0 p s i f r o m J room t e m p e r a t u r e t o 3OO0F, h e o b s e r v e d a r e d u c t i o n i n a b s o l u t e p e r m e a b i l i t y of as much as 65%. With m i n e r a l o i l flow, or i n e r t g a s f l o w , he found t h a t t e m p e r a t u r e had no a p p r e c i a b l e J e f f e c t on a b s o l u t e permeabilt i t y . Recently, Arihara2 r e p o r t e d t h a t i n h i s w a t e r f l o w e x p e r i m e n t s t h r o u g h s y n t h e t i c cementc o n s o l i d a t e d s a n d cores, h e d i d n o t o b s e r v e t e m p e r a t u r e J e f f e c t s on a b s o l u t e p e r m e a b i l i t y . However, h e a p p l i e d l o w confining pressures. Cassgl suggested t h a t clay- water i n t e r a c t i o n caused t h e permeability r e d u c t i o n he observed. I However, G r e e n b e r g , e t al. 4 i n 1 9 6 8 r e p o r t e d d a t a o n t h e p e r m e a b i l i t i e s t o w a t e r o f core samples a r t i f i c i a l l y c o n s o l i d a t e d w i t h p h e n o l i c r e s i n o r by sintering. J The g e n e r a l t r e n d showed s l i g h t t o moderate de- creases i n p e r m e a b i l i t y w i t h i n c r e a s i n g t e m p e r a t u r e . f i n i n g p r e s s u r e w a s a p p l i e d to the core. N o con- They a t t r i b u t e d t h e J observed changes t o m i c r o - s t r u c t u r a l re- arrangements i n t h e m a t r i x geometry of t h e sampl-es which had a rough and i r r e g u l a r surface. They o b s e r v e d no c h a n g e s i n p e r m e a b i l i t i e s f o r J samples w i t h r e l a t i v e l y smooth s u r f a c e s . The p u r p o s e of t h i s work w a s (1) t o v e r i f y t h e r e s u l t s of p r e v i o u s s t u d i e s , ( 2 ) t o e x t e n d t h e p r e v i o u s work t o o t h e r s y s t e m s , and ( 3 ) t o i n v e s t i g a t e t h e r e a s o n f o r t e m p e r a t u r e J i -2d -- I , e f f e c t s on a b s o l u t e p e r m e a b i l i t y . I n order t o provide a c l u e as t o what a c t u a l l y c a u s e d t h e p e r m e a b i l i t y t o d e c r e a s e w i t h i n c r e a s i n g t e m p e r a t u r e , it was d e c i d e d t o u s e c l a y - f r e e r o c k s and o t h e r p o l a r l . i q u i d s , such as 2 - o c t a n o l . \- I. c. c L -3- 2. FLOW IN POROUS WDIA I n 1 8 5 6 , as a r e s u l t of e x p e r i m e n t a l s t u d i e s on t h e f l o 7 of water t h r o u g h u n c o n s o l i d a t e d s a n d f i l t e r b e d s , Henry Darcyk f o r m u l a t e d a flow l a w which now b e a r s h i s name. T h i s l a w hag been extended t o d e s c r i b e , w i t h some l i m i t a t i o n s , t h e movemeqt of o t h e r f l u i d s , i n c l u d i n g t w o or more i m m i s c i b l e f l u i d s , i n c o n s o l i d a t e d r o c k s and 0 t h r p o r o u s media. 2.1 Darcy's' L a w Darcy's law, f o r t h e h o r i z o n t a l , v i s c o u s f l o w o f a f l u i d i n a l i n e a r medium, s t a t e s t h a t t h e flow v e l o c i t y of a homogeneous f l u i d i s p r o p o r t i o n a l t o t h e p r e s s u r e g r a d i e n t , and i n v e r s e l y p r o p o r t i o n a l t o t h e f l u i d v i s c o s i t y , or: (2- where v i s t h e v e l o c i t y i : n cm/sec, a_ i s t h e f l o w r a t e i n c c / sec, p i s t h e f l u i d v i s c o s i t y i n c p , d p / d s i s t h e p r e s s u r e gradient i n atm/cm, t a k e n i n t h e f i r e c t i o n o f f l o w , and k i s t h e rock permeability, d a r c i e s . A r o c k of one d a r c y p e r - m e a b i l i t y i s one i n which a f l u i d of o n e c e n t i p o i s e v i s c o s i t j w i l l move a t a v e l o c i t y o f o n e c e n t i m e t e r p e r second under a p r e s s u r e g r a d i e n t of o n e a t m o s p h e r e p e r c e n t i m e t e r . D a r c y ' s l a w a p p l i e s o n l y i n t h e r e g i o n of l a m i n a r f l o w . F o r " t u r b u l e n t " or n o n - l a m i n a r f l o w s which o c c u r a t h i g h e r velocities, the pressure gradient increases at a greater rate t h a n d o e s t h e flow r a t e . -4- A c o r r e l a t i o n produced by F a n c h e r , L e w i s , and Barnes 5 may b e used t o e s t i v a t e t h e r e p i o n of v i s c o u s flow f o r a p o r o u s medium. I n g e n e r a l , 9 a r c y ' s l a w is v a l i d f o r p o r o u s media when a m o d i f i e d Reynolds' number IJ R e = vd P i s less t h a n one. v i s v e l o c i t y , p i s f l u i d d e n s i t y , 1.1 i s t h e f l u i d v i s c o s i t y , and d i s t h e d i a m e t e r of t h e a v e r a g e grain size. A r e c e n t s t u d y by Geertsma' showed t h a t t h e a v e r a g e g r a i n s i z e s h o u l d b e r e p l a c e d by a r a t i o of p e r m e a b i l i t y t o ' ' porosity t o provide a b e t t e r correlation. The r e q u i r e m e n t t h a t t h e p e r m e a b i l i t y be d e t e r m i n e d for c o n d i t i o n s of v i s c o u s flow i s b e s t s a t i s f i e d 7 by o b t a i n i h g d a t a a t s e v e r a l flow rat:es and g r a p h i n e f l o w r a t e v e r s u s prtelss u r e d r o p f o r l i q u i d and f o r gas by p l o t t i n g t h e p r o d u c t of mean f l o w r a t e and p o r e p r e s s u r e v e r s u s p1 2 - ~ * p 2 where p1 , i s t h e u p s t r e a m p r e s s u r e and p 2 i s t h e downstream p r e s s u r e . For c o n d i t i o n s of v i s c o u s flow, t h e d a t a s h o u l d p l o t a s t r a i g h t l i n e , passing through t h e origin. Turbulence i s i n d i c a t e d I by c u r v a t u r e of t h e p l o t t e d p o i n t s . 2.2 D a r c y ' s Law f o r G a s Flow I n t h e case of f l o w of g a s e s , t h e f l o w r a t e i s n o t I constant, but increases with t h e pressure drop, according t o Boyle's l a w . T h e i n t e g r a t e d form o f D a r c y ' s l a w which d e s - c r i b e s h o r i z o n t a l l i n e a r . p a s flow, u n d e r s t e a d y s t a t e , i s o thermal c o n d i t i o n s i s : - 5- I i 2 (2-3) J 2.3 S l i p Phenomena i n G a s Flow Kundt and Warburg* f i i ~ s tshowed t h a t a l a y e r of g a s J n e x t t o a s o l i d s u r f a c e m!y h a v e a f i n i t e v e l o c i t y w i t h respect t o t h e w a l l . I n case o f c a p i l l a r y f l o w , t h i s would g i v e a g r e a t e r r a t e t h a n would b e computed f r o m P o i s e u i l l e ' s J law. I n e f f e c t , t h e g a s stream l l s l i p s " w i t h r e s p e c t t o t h e wall. T h i s i s n o t t h e case f o r l i q u i d f l o w . This "slip" phenomena i s d e p e n d e n t upon t h e mean f r e e p a t h of t h e g a s J molecules; t h e r e f o r e , gas permeability should b e a f u n c t i o n of t h e f a c t o r s c o n t r o l l i n g t h e mean f r e e p a t h . These f a c t o r s a r e p r e s s u r e , t e m p e r a t u r e , and t h e n a t u r e o f t h e g a s i t s e l f . When t h e mean f r e e p a t h s ar*e small, e . g . , 4 at high pressures, t h e p e r m e a b i l i t y t o g a s s h o u l d be e x p e c t e d t o a p p r o a c h t h a t t o liquids. T h i s i d e a w a s s u p p o r t e d by t h e K l i n k e n b u r g 9 J study. Based upon a t h e o r e t i c a l a n a l y s i s o f t h e s l i p phenomenon i n c i r c u l a r c a p i l l a r i e s , arid assuming a n a n a l o g o u s b e h a v i o r i n a p o r o u s medium, K l i n k e n b e r g ' J developed the r e l a t i o n s h i p between t h e p e r m e a b i l i t y of a p o r o u s medium t o g a s and t o a J n o n r e a c t i v e l i q u i d as follows: (2-411 .J I I. .J where ka i s t h e apparent: o r o b s e r v e d p e r m e a b i l i t y t o g a s , k i s t h e a b s o l u t e permeability t o gas a t h i g h pressures (presumed e q u a l t o t h e a b s o l u t e p e r m e a b i l i t y t o a s i n g l e l i q u i d - phase) ,X i s t h e mean fr5ee p a t h of t h e g a s m l e c u l e s , r i s t h e r a d i u s of a c a p i l l a x - y (assumed t o b e c o n s t a n t ) i s a proportionality factor. , and c The mean f r e e p a t h c a n b e e x p r e s s e d as: where d i s a c o l l i s i o n diameter, n i s t h e c o n c e n t r a t i o n of m o l e c u l e s p e r u n i t volume, N i s Avogadro's N u m b e r , p, i s the mean p r e s s u r e , T i s a b s o l u t e t e m p e r a t u r e , and R i s t h e u n i versa1 gas constant. k a ~ F ~ o mEa_. 2 - 5 , Eq. 2- 4 becomes: = k(l+- 4c'T ) = k(l+-)b 2 Pm m r N d pm c. where b i s r e f e r r e d t o as t h e K l i n k e n b e r g f a c t o r , and is u s u a l l y t a k e n as a c o n s t a n t f o r a g i v e n gas and a g i v e n c p o r o u s medium. From E q . 2 - 6 , t h e K l i n k e n b e r g f a c t o r appear\$ d i r e c t l y p r o p o r t i o n a l t o temperature. 2.4 V i s c o - I n e r t i a l F l o wD a r c y ' s l a w and t h e p r e c e d i n p e q u a t i o n s a r e v a l i d when c o n d i t i o n s of v i s c o u s f l o w p r e v a i l . A t h i g h flow r a t e s , f L b w has b e e n shown t o b e d e s c r i b e d by a q u a d r a t i c e q u a t i o n . a n e q u a t i o n was proposed by Forchheimer'' C o r n e l l a n d K a t z l l as f o l l o w s : -7- and m o d i f i e d by Su Dranchuk and Kolada12 have shown how t o d e l i n e a t e t h e v i s c o - i n e r t i a l f l o w r e g i o n from flow measurements, and how t o d e t e r m i n e t h e a b s o l u t e p e r m e a b i l i t y of a r o c k c o r e ( s e e Appendix 9 . 3 ) . 2-7 is some- The v i s c o - i n e r t i a l f l o w d e s c r i b e d by E q . t i m e s r e f e r r e d t o as " t u r l b u l e n t " flow. The d e p a r t u r e from J l a m i n a r flow d e s c r i b e d by E q . 2- 7 i s n o t c a u s e d by physical f a c t o r s which (cause t u r b u l e n t flow i n p i p e . i s u s u a l l y r e f e r r e d t o as "non-Darcy," i n e r t i a l " flow. T h i s phenomenon I " i n e r t i a l , " or "visco-r W e s h a l l u s e t h e l a t t e r term. J I I J J J J Y I -8- .J .. LITE-WTURE 3. I n 1 9 3 7 , Muskat4 s t a t e d t h a t t h e a b s o l u t e p e r m e a b i l i t y of a porous medium " i s t h u s a c o n s t a n t d e t e r m i n e d o n l y by t h e s t r u c t u r e of t h e medium i n q u e s t i o n and i s e n t i r e l y i n d e t pendent of t h e n a t u r e o f t h e f l u i d . " Also, t h e standard p r a t c e d u r e f o r d e t e r m i n i n g t h e p e r m e a b i l i t y of p o r o u s medium a c c o r d i n g t o A P I Code No. 2 7 1 5 ( f i r s t e d i t i o n , October 1935) w a s based on t h e f u n d a m e n t a l a s s u m p t i o n t h a t as l o n g as t h e r a t e of flow w a s p r o p o r t i o n a l t o t h e p r e s s u r e g r a d i e n t , t h e I p e r m e a b i l i t y c o n s t a n t of a p o r o u s medium w a s a p r o p e r t y of ~ t h e medium and w a s i n d e p e n d e n t o f t h e f l u i d used i n i t s detdLmination. A major s t u d y by K l i n k e n b e r g appeared i n 1 9 4 1 . ... Klinkefi- b e r g 9 performed l i q u i d p e r m e a b i l i t y measurements on J e n a f i l t e r s i n order t o avoid c l a y swelling o r erosion. The were n o t c o n f i n e d n o r w e r e v a r i a t i o n s i n t e m p e r a t u r e studiedl. From h i s a n a l y s i s o f gas, f l o w t h r o u g h t h e same c o r e s , he t h e p e f o r e supported t h e n o t i o n t h a t t h e permeability c o n s t a n t of a porous medium w a s a p r o p e r t y of t h e medium, and w a s i n d e p e n - dent of t h e f l u i d used. I n a d d i t i o n , he w a s t h e f i r s t persdn ~ t o e x p l a i n s l i p phenomena. I n 1 9 4 3 , Grunberg and N i s s a n 1 3 s t u d i e d t h e e f f e c t of f l o w of aqueous s o l u t i o n s t h r o u g h l i m e s t o n e and s a n d s t o n e c o r e s o v e r a r a n g e of t e m p e r a t u r e s . -9- Four s o l u t i o n s w e r e t e s t e d : (1) d i s t i l l e d water, (2) a 2 % n-amyl a l c o h o l s o l u t i o n , and ( 3 ) two s o d i u m c h l o r i d e s o l u t i o n s ( 0 . 9 6 0 and 0.614N). The c h o i c e o f t h e s e s o l u t i o n s was made s o as t o o b s e r v e t h e i n f l u e n c e o f s u r f a c e f o r c e s on t h e f l o w of l i q u i d s t h r o u g h p o r o u s media. The core t e m p e r a t u r e s were v a r i e d from 6OC I t o 3OoC. 1 Pe rmeab i1.it y d ecr e a:; e d w i t h i n c r e as ing t e m p e r a t u r e f o r a l l of t h e four, aqueous s o l u t i o n s . 1 1 A l l f o u r gave l i n e a r p e r m e a b i l i t y t e m p e r a t u r e c u r v e s w i t h a p p r o x i m a t e l y t h e same 1 The slope of t h e g r a p h s o f p e r m e a b i l i t y v s . tempera- slope. t u r e w a s 0 . 8 mcV0C. Thus: k = if - ( 3-1 0.8(t,OC) I where a i s a c h a r a c t e r i s t i c c o n s t a n t o f t h e l i q u i d used. As t h e f l u i d v i s c o s i t y w a s considered properly i n c a l c u l a t i n g ~ I p e r m e a b i l i t y , t:hey concluded t h a t v i s c o s i t y w a s n o t t h e o n l y p r o p e r t y i n f l u e n c i n g flow. 1 I n a d d i t i o n , a l o g - l o g g r a p h of 2 I k/k ,vs.(-) lJ g a v e a s t r a i g h t l i n e . kl i s a base p e r m e a b i l i t y ; 1 Pa 1.1 i s f l u i d v i s c o s i t y , p i s f l u i d d e n s i t y , and Q i s s u r f a c e 1 tension. A c o n c l u s i o n reached w a s t h a t the e f f e c t i v e c r o s s - s e c t i t under v i s c o u s flow was d i f f e r e n t f o r d i f f e r e n t l i q u i d s due ti d i f f e r e n c e s i n s u r f a c e e n e r g y , and t h u s d i f f e r e n c e s i n t h e t h i c k n e s s of a d s o r b e d l a y e r s . I n 1 9 4 6 , Calhoun and Y u s t e r " p r e s e n t e d r e s u l t s of flow t h r o u g h a r t i f i c i a l p o r o u s b o d i e s , some made of p y r e x g l a s s and o t h e r s of f'used q u a r t z . No c o n f i n i n g p r e s s u r e was a p p l i e -10- I L They d i s a g r e e d w i t h G r u n b e r g ' s and N i s s a n ' s r e s u l t s and confirmed Klinkenberg's r e s u l t s . Calhoun a n d Y u s t e r found t h a t water g a v e a s l i g h t l y lower v a l u e for p e r m e a b i l i t y t h a n b e n z e n e . A s u s p i c i o n of a n e l e c t r o - k i n e t i c e f f e c t w a s r u l e d o u t b e c a u s e a d d i t i o n of a t r a c e of H C 1 or C a C 1 2 t o t h e water c a u s e d no a p p a r e n t i n crease i n p e r m e a b i l i t y . c. F u r t h e r m o r e , n a p h t h a gave a permea- b i l i t y as low as t h a t of w a t e r , a n d , w i t h this h y d r o c a r b o n l i q u i d a n e l e c t r o - k i n e t i c e f f e c t should have been a b s e n t . Calhoun and Y u s t e r were unable t o g i v e an e x p l a n a t i o n of c. t h i s anomaly. They were t h e f i r s t t o o b s e r v e a dependency od K l i n k e n b e r g ' s f a c t o r , b on t e m p e r a t u r e . 1 I n t r y i n g t o correlate Klinkenberg b values a t d i f f e r e n t c. t e m p e r a t u r e s , Calhoun and Y u s t e r assumed t h a t e q u a l mean fred I p a t h s would o c c u r a t e q u i v a l e n t m o l e c u l a r c o n c e n t r a t i o n s a t d i f f e r e n t temperatures, . , A g a s a t p r e s s u r e p1 and T1 s h o u l d ~ h a v e t h e same m o l e c u l a r c o n c e n t r a t i o n as t h e same g a s a t a p r e s s u r e p z a n d T2, i f P:1 ~1 were equal t o p2 T . Therefore, e q u i jI 2 v a l e n t p e r m e a b i l i t y v a l u e s s h o u l d e x i s t f o r t h e same g a s , whcin . two d i f f e r e n t t e m p e r a t u r e s were u s e d , a t a mean p r e s s u r e p, T1 and t e m p e r a t u r e T1, and a t mean p r e s s u r e p (-1 a t a temperad T2 t u r e of Tz. c ' This correLation at d i f f e r e n t temperatures w a s n o t i n c l u d e d i n e i t h e r K l i n k e n b e r g ' s or Grunberg and Nissan'B presentation. I n t h e l a t e 1960s, Greenberg, e t a1.,3 and Weinbrandt 18 a g a i n o b s e r v e d a p e r m e a b i l i t y dependency on t e m p e r a t u r e l e v e a . G r e e n b e r g , e t a l . , d i d n o t r e s t r a i n t h e i r cores and o b s e r v e d -11- i I J o n l y small t e m p e r a t u r e e f f e c t s . Weinbrandt 16 , in h i s experi- ments on t h e e f f e c t of t e m p e r a t u r e on r e l a t i v e and a b s o l u t e p e r m e a b i l i t y of s a n d s t o n e s , s u b j e c t e d h i s cores t o 2 0 0 0 p s i confining pressure. J H e a l s o f i r e d t h e cores a t 94OoF p r i o r I t o u s e t o o x i d i z e o r g a n i c matter i n t h e cores and t o d e a c t i - ' vate the clays. H i s e x p e r i m e n t s f o r B o i s e s a n d s t o n e core J s a m p l e s a t room t e m p e r a t u r e and a t 175OF showed t h a t w i t h a n increase i n temperature: (1) t h e i r r e d u c i b l e water s a t u r a t i o f a J increased; ( 2 ) t h e r e s i d u a l o i l s a t u r a t i o n decreased; ( 3 ) t h e r e l a t i v e permeability t o w a t e r a t flood- out increased; ( t h e r e l a t i v e perrneabi1it:y t o o i l i n c r e a s e d ; ( 5 ) t h e r e l a t i v e J p e r m e a b i l i t y i q a t i o , kw/ko, d e c r e a s e d ; and ( 6 ) t h e a b s o l u t e p e r m e a b i l i t y to w a t e r d e c r e a s e d . 1 v e r i f i e d t h e WeinCasse. I b r a n d t f i n d i n g s and s u b s t a n t i a l l y e x t e n d e d t h e work. J The e f f e c t of m e c h a n i c a l stresses on t h e p e r m e a b i l i t y of r o c k s has h e e n s t u d i e d b y s e v e r a l i n v e s t i g a t o r s . I n 196711 I I Wilhelmi and Somerton17 i n v e s t i g a t e d t h e e f f e c t of overburdefl 1 p r e s s u r e on r o c k p e r m e a b i l i t y . J They c o n f i r m e d e a r l i e r work b y F a t t and D a v i s 1 8 i n 1!352, and r e p o r t e d t h a t p e r m e a b i l i t y ' a t 1 5 , 0 0 0 p s i c o n f i n i n g p r e s s u r e c o u l d be 2 5 t o 6 0 % smaller J t h a n t h e permeability a t a z e r o c o n f i n i n g p r e s s u r e , dependin PP I t o n t h e t y p e of r o c k s s t u d i e d . Generally speaking, t h e h i g h e l t h e permeability, t h e higher t h e percentage of reduction. J About 6 0 % of t h e t o t a l r e d u c t i o n o c c u r r e d d u r i n g t h e f i r s t 3000 p s i confining p r e s s u r e . In 1963!, G r a y , --e t a1 ,19 a l s o measured t h e e f f e c t of o v e r b u r d e n p r e s s u r e on p e r m e a b i l i t y . ~ I I J Perneability reduction was shown t o be a f u n c t i o n of t h e r a t i o of r a d i a l t o a x i a l - 12- J s t r e s s , w i t h t h e maximum r e d u c t i o n o c c u r r i n g u n d e r a u n i f o r m stress, i . e . , stress. when t h e a x i a l stress i s e q u a l t o t h e r a d i a l The p r e s e n t work r e p o r t e d h e r e w a s accompanied undeth c o n d i t i o n s of u n i f o r m s t ~ e s s . Zoback and B y e r l e e (1975aI2' showed t h a t d u e t o t h e p r e s e n c e of c o m p r e s s i b l e m a t r i x material i n a r e l a t i v e l y i n c o m p r e s s i b l e g r a n u l a r framework, t h e p e r m e a b i l i t y o f s a n d s t o n e i s n o t simply a f u n c t i o n of e f f e c t i v e stress, b u t i s ~ highly s e n s i t i v e t o changes i n pore p r e s s u r e . The e f f e c t of t h e r m a l stresses on r o c k p r o p e r t i e s a n d t h e e f f e c t of o v e r b u r d e n p r e s s u r e on p o r o s i t y h a v e a l s o b e e n of p a r t i c u l a r i n t e r e s t . Somerton, e t a l . , * ' L h e a t e d a number of s a n d s t o n e s t o a b o u t 150OOF u n d e r b o t h a t m o s p h e r i c and s i m u l a t e d r e s e r v o i r pressures. P e r m e a b i l i t y w a s measured a t room t e m p e r a t u r e u s i n g a s t a n d a r d a i r perimeameter, b e f o r e and a f t e r h e a t i n g t h e samples. I No p e r m e a b i l i t y c h a n g e s were r e p o r t e d i n t h e r a n g e of 75-350°F. A t t e m p e r a t u r e s w e l l a b o v e 5OO0F, t h e y showed t h a t permanent s t i r u c t u r a l damage and d e c o m p o s i t i o n ofi1 r o c k minerals o c c u r r e d d u e t o thermal stresses. Wyble22, w o r k i n g om t h e e f f e c t o f a p p l i e d p r e s s u r e on s a n d s t o n e ' s p r o p e r t i e s , o b s e r v e d a s y m p t o t i c d e c r e a s e s i n cond u c t i v i t y , p o r o s i t y , and p e r m e a b i l i t y o v e r a 0 p s i t o 3,500 p s i range. A t 2000 p s i c o n f i n i n g p r e s s u r e , about a 10% reduc- t i o n i n p o r o s i t y w a s obslerved, and beyond t h i s , t h e p o r o s i t y v a l u e remained e s s e n t i a l l y c o n s t a n t . -13- I n s u m m r y , many s t u d i e s i n d i c a t e t h e l i k e l i h o o d of a b s o l u t e p e r m e a b i l i t y of r o c k s b e i n g a f u n c t i o n o f t e n p e r a - t u r e beyond t h e e f f e c t s c a u s e d b y a c h a n g e i n t h e v i s c o s i t y I of t h e f l u i d . The r e c e n t works of Weinbrandt’‘ and Cass6 1 1 i n d i c a t e d an e f f e c t o f major i m p o r t a n c e for r e s t r a i n e d c o r e s 4 N o obvious explanation existed. The main p u r p o s e of t h i s I s t u d y w a s a v e r i f i c a t i o n of and s t u d y o f p o s s i b l e e x p l a n a t i o o s 1 of t h e s e e f f e c t s . I -14- i 4. EXPERIMENTAL EQUIPMENT The e x p e r i m e n t a l eciuipment used w a s s i m i l a r t o t h a t .. d e s c r i b e d p r e v i o u s l y by Cass6’ and Weinbrandt 1 6 . f i c a t i o n s were made i n t h e a p p a r a t u s , however. Some modi- 1 A description of t h e a p p a r a t u s f o l l o w s . I I. 4.1 General Descriptioh F i g . 1 i s a photogriaph of t h e l a b o r a t o r y , and F i g . 2 p r e s e n t s t h e d e t a i l s of t h e a i r b a t h assembly. diagram o f t h e a p p a r a t u s i s shown i n F i g . 3. A schematic T h e flow l i n e s , h e a t e x c h a n g e r s , and f i t t i n g s were c o n s t r u c t e d o f 316 s t a i n l e 6S s t e e l material. c. Three p a r a l l e l flow l i n e s were c o n s t r u c t e d for- g a s , o i l , water, or 2 - o c t a n o l i n j e c t i o n . For e a c h e x p e r i m e n t , t h e 1 d e s i r e d f l o w l i n e w a s c o n n e c t e d t o t h e c o r e ; a new c o r e b e i n g used f o r e a c h e x p e r i m e n t . Liquid flow w a s s u p p l i e d by a p u l - s a t i n g pump, and gas f l o w w a s s u p p l i e d f r o m h i g h p r e s s u r e c y l i n d e r s and d e l i v e r e d t‘hrough p r e c i s i o n p r e s s u r e r e g u l a t o r s . L i q u i d f l o w r a t e th:rough t h e c o r e w a s measured by a weighing b a l a n c e . Depe:nding upon t h e l e v e l of f l o w r a t e , gas flow r a t e w a s measured e i t h e r by t h e use of a b u b b l e f i l m 1 flowmeter o r by a Wet T e s t Meter. A thermocouple w a s placed a t t h e i n l e t f a c e of t h e c o r e , and t e m p e r a t u r e w a s r e c o r d e d continuously during t h e runs. The c o r e h o l d e r a s s e m b l y was p l a c e d i n an air b a t h t h a t maintained r u n t e m p e r a t u r e . Mea- s u r e m e n t s of u p s t r e a m p r e s s u r e and p r e s s u r e d r o p across t h e -15- f i !I. 1. PhotoF,raph o f A p p a r a t u s I c. W - 17- I I I I c o r e were a c c o m p l i s h e d by t h e u s e of p r e s s u r e t r a n s d u c e r s connected t o p r e s s u r e i n d i c a t o r s and r e c o r d e r s . The d e s i r e d c o n f i n i n g p r e s s u r e l e v e l was a t t a i n e d by u s i n g a h y d r a u l i c hand pump. Chevron No. 15 h e a v y O i l was used as a c o n f i n i n g f l u i d and a " V i t o n A" r u b b e r s l e e v e , J l / S " t h i c k , s e p a r a t e d t h i s f l u i d from t h e core. I A d e s c r i p t i o n of t h e major components o f t h e a p p a r a t u s follows. 4.2 Core H o l der - -_ F i g . 4 s ' h o w s t h e d e t a i l s of t h e c o r e h o l d e r which i s a Hassler r u b b e r sleeve t y p e . The r o c k specimen t o be s t u d i e d i s h e l d i n a " V i t o n A" r u b b e r s l e e v e , 1/8" t h i c k , between a n u p s t r e a m p l u g , which i s immobile, and a downstrean p l u g which moves h o r i z o n t a l l y and a d j u s t s t o t h e core l e n g t h . The u p s t r e a m p2ug h a s two p r e s s u r e t a p s A and D , one tap B f o r i n l e t f l o w : , and a t h e r m o c o u p l e w e l l C . E i t h e r l i q u i d o r g a s p r e s s u r e c a n be a p p l i e d t o t h e Viton s l e e v e , b u t thrloughout t h e s e e x p e r i m e n t s , Chevron White O i l No. 1.5 w a s u s e d . Both a x i a l and r a d i a l c o n f i n i n g p r e s s u r e s are a.pplied s i m u l t a n e o u s l y t o t h e core b e c a u s e t h e downstream plug, i s m o b i l e and s u b j e c t t o t h e c o n f i n i n g p r e s sure. A p e r f o r a t e d aluminum t u b e i s f i t t e d around t h e core rubber s l e e v e t o p r e v e n t l a t e r a l deformation of core d u r i n g loading. The s l e e v e w a s 1 . 9 4 6 i n . OD by 3 . 0 i~ t h i c k c y l i n d e r 1 . 2 2 5 i n . I D by i n . long. I 4.3 A i r Bath and T e m p e r a t u r e C o n t r o l J An a i r b a t h w i t h a w o r k i n g s p a c e of 2 4 c u b i c f e e t housed t h e core h o l d e r a s s e m b l v . -18- Four kilowatts of power may .d NO- Icy 9 w o o 00 00 .- 0 0. , - a . a+ * I + Ex 1 I a 1 be a p p l i e d t o t h e h e a t i n g e l e m e n t s by a n A P I model 4010 power pack and a n API model. 2 2 8 t e m p e r a t u r e c o n t r o l l e r . The t h e r m o c o u p l e t h a t c o n t r o l s t h e o u t p u t o f the h e a t e r c o n t r o l l e r ~ c a n b e p l a c e d a t any l o c a t i o n i n s i d e t h e o v e n , b u t t h e most e f f i c i e n t h e a t i n g c y c l e w a s found t o r e s u l t when t h e thermoc o u p l e s e n s o r w a s f a s t e n e d t i g h t l y t o t h e core h o l d e r . A fan I I p r o v i d e d a d e q u a t e a i r c i r c u l a t i o n and t h e a i r b a t h w a s equipped' w i t h a l i g h t and a window. ~ Temperature was monitored by a 2 4 - p o i n t thermocouple r e c o r d e r w i t h i r o n - c o n s t a n t an t h e r m o c o u p l e s were a c t u a l l y used. . I Two thermocouple$' One thermocouple measured t h e t e m p e r a t u r e o f t h e c o r e , and t h e o t h e r measured t h e a i r b a t h t e m p e r a t u r e . The a i r b a t h t e m p e r a t u r e r e a c h e d t h e d e s i r e d t e s t t e m p e r a t u r e i n a b o u t 1 - 1 / 2 h o u r s , b u t a.t l e a s t a n o t h e r four h o u r s were r e q u i r e d f o r t h e r o c k specimen t o r e a c h t h e t e s t t e m p e r a t u r e . 4.4 - L i q u i d and Gas' Sources A d e a e r a t e d l i q u i d was s t o r e d i n a 4 0 0 0 cc c a p a c i t y vacuum f l a s k . A Lapp "Microflo" P u l s a f e e d e r pump w a s used t o pump t h e l i q u i d t h r o u g h t h e c o r e . The pump h a s a d i a l i n d i c a t o r , c a l i b r a t e d i n 1 0 0 0 i n c r e m e n t s which e n a b l e d f i n e a d j u s t m e n t s i n f l o w r a t e t o be made. Three t y p e s of l i q u i d s w e r e u s e d : w a t e r , o i l , and 2 - o c t a n o l . Gas flow t h r o u g h t h e samples w a s s u p p l i e d from h i g h p r e s s u r e c y l i n d e r s , and r e g , u l a t e d by a t w o - s t a g e a d j u s t - a b l e r e g u l a t o r equipped w i t h a r e l i e f v a l v e . The i n i t i a l c y l i n d e r p r e s s u r e w a s 2 5 0 0 p s i , and d e l i v e r y p r e s s u r e s ranged from 5 p s i t o a maximum o f 4 0 0 p s i . -20- I c 4.5 L i q u i d Pumps The pumps w e r e a Lapp "Microflo" P u l s a f e e d e r t y p e w i t h a d i a l i n d i c a t o r c a l i b r a t e d i n 1000 increments. Both pumps I created l a r g e p r e s s u r e p u l s a t i o n s when d e l i v e r i n g a t h i g h I pressures. Accumulators, i n s e r t e d a l o n g t h e f l o w l i n e s , eliminated t h e s e pulsations. I A steady flow could b e estab- l i s h e d and c o n s t a n t p r e s s u r e s m a i n t a i n e d a t b o t h e n d s o f the core. 4.6 H y d r a u l i c Yand P u r 2 An E n e r p a c h v d r a u l - i c hand pump w i t h a r a n g e of 0 t o 1 0 , 0 0 0 p s i provided adjustment o f t h e c o n f i n i n g p r e s s u r e . The pump w a s c o n n e c t e d to t h e c o r e h o l d e r and Chevron White M i n e r a l O i l No, 1 5 was used t o o b t a i n t h e d e s i r e d c o n f i n i n g pressure. 4.7 Heat E x c h a n g e r s To m a i n t a i n t h e t e m p e r a t u r e o f t h e f l o w i n g f l u i d conI s t a n t d u r i n g a r u n , l a r g e r e s e r v o i r s were i n s t a l l e d on each1 f l o w l i n e i n s i d e t h e oven b e f o r e t h e c o r e h o l d e r . e n t e r e d a t t h e bottom of t h e r e s e r v o i r . Cold flu1 Because o f t h e larj s i z e o f t h e r e s e r v o i r arid t h e s m a l l flow r a t e s that were I used w i t h l i q u i d f l o w , h o t f l u i d l e f t from t h e t o p . The t e m p e r a t u r e o f t h e l i q u i d s l e a v i n g t h e r e s e r v o i r and e n t e r i d g I t h e c o r e w a s measured and found t o remain c o n s t a n t a t t h e 1 I I d e s i r e d test t e m p e r a t u r e d u r i n g t h e e n t i r e r u n . The g a s r e s e r v o i r i n s i d e t h e oven w a s f i l l e d w i t h s t a i n I l e s s s t e e l wool. T h i s improved h e a t exchange and e n a b l e d t h e gas t o r e a c h t h e t e s t t e m p e r a t u r e b e f o r e e n t e r i n g t h e c b r e . -21- The e f f l u e n t f r o m t h e c o r e and t h e a i r b a t h w a s c o o l e d p r i o r t o f l o w rate determination. This w a s accomplished by l e t t i n g t h e e f f l u e n t flow t h r o u g h a c o i l immersed i n a con- ~ s t a n t room t e m p e r a t u r e water b a t h . 4.8 Backpressure Valve B a c k p r e s s u r e was r e g u l a t e d by means of a f i n e m e t e r i n g needle valve. T h i s v a l v e , i n a d d i t i o n t o b e i n g used t o c h a n g e I/ I t h e f l o w r a t e , served t o maintain a s u f f i c i e n t l y high pressure i n t h e s y s t e m t o keep t h e o p e r a t i n g l i q u i d i n t h e l i q u i d state. I I By a d j u s t i n g t h e v a l v e and t h e pump r a t e , a c o n s t a n t i mean p o r e p r e s s u r e could b e m a i n t a i n e d . M a i n t a i n i n g a con- s t a n t mean p o r e p r e s s u r e l e v e l w a s i m p o r t a n t because e x p e r i m e n t a l work by Zoback*' , showed t h a t a change i n mean pore p r e s s u r e c o u l d a f f e c t a b s o l u t e p e r m e a b i l i t y t o an even g r e a t e r e x t e n t t h a n d i d a change i n c o n f i n i n g p r e s s u r e . A constant , mean p o r e p r e s s u r e of 2 0 0 p s i w a s m a i n t a i n e d f o r a l l l i q u i d runs. 4.9 Flow Rate Measuring D e v i c e s l i 4.9- 1 Liquid F l o w : A t s t e a d y s t a t e , t h e mass f l o w r a t e w a s c o n s t a n t t h r o u g h o u t t h e system. The mass f l o w r a t e w a s measured by weighing small volumes o f t h e e f f l u e n t l i q u i d by a n a n a l y t i c a l b a l a n c e o v e r a known p e r i o d of trime. Repeated measurement p e r m i t t e d c h e c k i n g d e t e r m i n a t i o n of s t e a d y s t a t e . T h e v o l u m e t r i c flow r a t e w i t h i n t h e c o r e was determined as t h e ratio of t h e mass flow ]?ate t o t h e d e n s i t y of t h e l i q u i d a t r u n t e m p e r a t u r e and mean p r e s s u r e . - 2 2- The flow r a t e c o u l d be changed by a d j u s t i n g t h e pump r a t e a n d / o r by a d j u s t i n g t h e needle valve. 4.9- 2 Gas Flow: Gas p r e s s u r e w a s r e g u l a t e d u p s t r e a m by a two- stage p r e s s u r e r e g u l a t o r and g a s flow w a s r e g u l a t e downstream by means of a n e e d l e v a l v e . T h e c h o i c e of t h e I a p p r o p r i a t e flowmeter w a s made a c c o r d i n g t o t h e l e v e l o f f l i . e . , l a m i n a r flow (low r a t e ) , or v i s c o - i n e r t i a l flow ( h i g h rate). A b u b b l e f i l m flowmeter w a s u s e d for a l l l a m i n a r f l measurements and a Wet T e s t Meter was used f o r v i s c o - i n e r t : f l o w measurements. L 0.2 A s t o p watch, graduated i n d i v i s i o n s of second, w a s used as a t i m i n g d e v i c e . I The bubble f i l m flowmeter w a s t h e m o s t a c c u r a t e o f t h $ / 1 two d e v i c e s , and was used t o check t h e Wet T e s t Meter a t lod flow r a t e s . The b u b b l e f i l m flowmeter w a s made as follows. I The v e r t i c a l p a r t of a Y-shaped t u b e i s plunged j u s t up t o t h e t h r o a t i n a s o a p s o l . u t i o n (see F i g . 1). The g a s f l o w I t o b e metered e n t e r s t h r o u g h one of t h e b r a n c h e s and bubble$' i n t o t h e o t h e r b r a n c h arid t h e n up i n t o t h e v e r t i c a l b u r e t t e The flow r a t e i s o b t a i n e d by m e a s u r i n g t h e t i m e it t a k e s f o a b u b b l e t o t r a v e r s e a known volume i n t h e b u r e t t e . This method e s s e n t i a l l y provj-ded f l o w r a t e measurements a t room c o n d i t i o n s because t h e p r e s s u r e r e q u i r e d t o d i s p l a c e t h e b u b b l e s was always less t h a n 0 . 0 1 p s i . 4.10 P r e s s u r e Recording D e v i c e s Upstream p r e s s u r e and p r e s s u r e d r o p a c r o s s t h e c o r e w e r e measured w i t h a Pace Model KP15 d i f f e r e n t i a l p r e s s u r e -23- I J t r a n s d u c e r and a Pace '-%del C D 2 5 t r a n s d u c e r i n d i c a t o r . The a p p r o p r i a t e p l a t e (1 p s i , 5 p s i , 2 5 p s i , 1 0 0 p s i , o r 500 p s i ) J w a s u s e d f o r t h e working r a n g e of pressure o r p r e s s u r e d r o p . An e l e c t r o n i c two-pen mult i - r a n g e r e c o r d e r , " C h e s s e l l ,I' was c o n n e c t e d t o t h e i n d i c a t o r and p r o v i d e d a permanent r e c o r d of t h e p r e s s u r e . A B a r n e t t Dead Weight T e s t e r w a s used t o c a l i b r a t e t h e pressure recording devices. I J l i J .J 'i - -24- 5. PROCEDURE Core s a m p l e s t o b e s t u d i e d were h e l d , c o m p l e t e l y sat&a t e d w i t h t h e d e s i r e d l i q u i d , i n a Hassler, r u b b e r s l e e v e t y p e c o r e h o l d e r , i n an a i r b a t h . The t e m p e r a t u r e of t h e air b a t h and t h a t o f t h e c o r e were t h e n b r o u g h t t o t h e d e s i r e d Flow w a s e s t a b l i s h e d , and a f t e r r e a c h i n g a s t e a d y - level. I s t a t e c o n d i t i o n , t h e n e c e s s a r y p r e s s u r e measurements and f l b w r a t e s were measured. With t h e n e c e s s a r y c o r r e c t i o n s f o r thlh I L e f f e c t o f t e m p e r a t u r e on f l u i d v i s c o s i t y and d e n s i t y , absol u t e p e r m e a b i l i t y o f t h e c o r e w a s computed a t run t e m p e r a t The l i q u i d s u s e d were water, Chevron White O i l N o . octanol. 5.1 3 , and 2 N i t r o g e n was t h e gas used. II Core P r e p a r a t i o n The t w o t y p e s of ‘rocks used i n t h i s s t u d y were c o n s o l I d a t e d M a s s i l l o n S a n d s t o n e s , and u n c o n s o l i d a t e d O t t a w a S i l i c h Sand. i.e., With t h e e x c e p t i o n o f t h e f i r s t run w i t h e a c h t y p e , 2 and No. 1 4 , t h e cores were f i r e d f o r experiments No. a t l e a s t 1 2 h o u r s i n a 5OO0C f u r n a c e s o as t o o x i d i z e any o r g a n i c matter p r e s e f i t 5.1- 1 . Consclidated Massillon Sandstones : The c o r e s were c u t w i t h a o n e - i n c h d i a m e t e r diamond d r i l l , trimmed on a l a t h e , e x t r a c t e d i n a Dean S t a r k t y p e a p p a r a t u s , and i g n i y e d i n a 5OO0C f u r n a c e . F u l l d e t a i l s o f t h e p r o c e s s are g i v e n i n Ref. 1. - 25- 2 A f t e r i g n i t i o n , thle c o r e s were s a t u r a t e d under vacuum w i t h t h e d e s i r e d flowing l i q u i d . T h e d i f f e r e n c e i n weight J a t 1 0 0 % l i q u i d s a t u r a t i o n and a t o t a l l y d r y c o n d i t i o n w a s used t o c a l c u l a t e t h e c o r e p o r o s i t y . For n i t r o g e n f l o w , t h e a i r - s a t u r a t e d c o r e w a s mounted II i i n t h e core h o l d e r and f l u s h e d w i t h s e v e r a l p o r e volumes of nitrogen. I I D e t a i l s of t h e p h y s i c a l and m i n e r a l o g i c a l p r o p e r t i e s 1 ~ of t h e s e c o r e s a p p e a r i n Appendix 9 . 2 . 5.1- 2 i I U n c o n s o l i d a t e d O t t a w a Sand: The sand was s i e v e d 1j and s e p a r a t e d i n t o uniforbmly g r a d e d s i z e s . For o n e run, ex- b u t r e t a i n e d i n s i e v e No. 4 5 w a s u s e d . J 35 p e r i m e n t No. 1 4 , t h e sand t h a t p a s s e d t h r o u g h s i e v e N o . F o r all t h e o t h e r r u n s , t h e sand s i z e t h a t p a s s e d t h r o u g h s i e v e No. 8 0 b u t was , d r e t a i n e d i n s i e v e No. 1 0 0 w a s used. T h i s g i v e s a v e r a g e sand I g r a i n s i z e s of 0.385 mm and 0.156 rrun r e s p e c t i v e l y . The I ! s a n d w a s i g n i t e d a t 50OoC. 4 T h e upstream p l u g was i n s e r t e d i n t o t h e r u b b e r s l e e v e and '1 t i g h t l y t i e d t o it w i t h 2 0 gage s t a i n l e s s s t e e l w i r e . 11 The c o r e l o a d i n g and assembly p r o g r a m w a s as follows: With t h e assembly h e l d v e r t i c a l l y u p r i g h t , a No. 4 0 0 s t a i n l e s s 4 I s t e e l mesh, one i n c h i n d i a m e t e r , w a s s e a t e d on t h e u p s t r e a m p l u g , and t h e sand w a s poured i n t o t h e s l e e v e slowly. When t h e s a n d was a b o u t 2 i n c h e s h i g h i n t h e s l e e v e , a n o t h e r I I Y s i m i l a r mesh w a s p l a c e d on t o p of s a n d pack and t h e downI stream p l u g was i n t r o d u c e d and a l s o f a s t e n e d i n t h e same manner. ~ 3 The assembly w a s t h e n p l a c e d i n t h e core h o l d e r and -26u a g a i n w e l l compacted and t i g 5 t e n e d w i t h t h e h e l p o f a v i c e . The f i n a l o v e r a l l measurtenent o f t h e c o r e h o l d e r w a s used t o c a l c u l a t e t h e a c t u a l l e n g t h of t h e c o r e i n p l a c e . The d i a m e t e r of t h e c o r e w a s t h e same as t h a t of t h e end p l u g s ( 1 - i n c h diameter). With t h e core h o l d e r p l a c e d i n t h e a i r b a t h and conn e c t e d t o t h e flow l i n e , t h e c o r e and t h e f l o w l i n e were c o m p l e t e l y e v a c u a t e d and, w h i l e under vacuun?, f l o w w a s s t a r d k d s o as t o c o m p l e t e l y s a t u r a t e t h e c o r e and f i l l t h e l i n e s w i t l the liquid. 1 I The d e t a i l s of t h e p h y s i c a l and m i n e r a l o g i c a l p r o p e r t i e s o f t h e s e c o r e s a l s o a p p e a r i n Appendix 9 . 2 . 5.2 E s t a b l i s h i n g Run C o n d i t i o n s With t h e core i n t h e c o r e h o l d e r , t h e e n t i r e asserrbly w a s p l a c e d i n a c r a d l e i n t h e a i r b a t h and a l l n e c e s s a r y c o n n e c t i o n s w e r e made t o t h e flow l i n e s , p r e s s u r e t a p s , and c o r e temperature probe. C o n f i n i n g p r e s s u r e w a s t h e n a p p l i e d s l o w l y by pumping Chevron White O i l N o . 1 5 around t h e c o r e s l e e v e , care b e i n g t a k e n t o d i s p l a c e a l l t h e a i r i n t h i s l i n e by o p e n i n g t h e 1 c o r e end o f t h e l i n e d u r i n g t h e i n i t i a l s t a g e o f pumping. A decreasing confining pressure with t i m e u s u a l l y indicated l e a k a g e o f t h e c o n f i n i n g f l u i d i n t o t h e c o r e and flow s y s t e m , To a v o i d l e a k a g e , a 2 0 gage s t a i n l e s s s t e e l w i r e w a s always t i e d around t h e r u b b e r s l e e v e between t h e end p l u g s and t h e r o c k b e f o r e assembly. A i r t h a t might have been t r a p p e d i n t h e c o r e and t h e flow s y s t e m w a s removed by c o n n e c t i n g a vacuum pump t o -27- t h e o u t f l o w end of t h e s y s t e m , a n d a p p l y i n g vacuum f o r a t l e a s t f i v e hours. Before t h e vacuum pump w a s d i s c o n n e c t e d , f l o w w a s s t a r t e d s o t h a t t h e whole s y s t e m w a s c o m p l e t e l y f i l l e d w i t h t h e l i q u i d t o be used. The assembled system w a s t h e n h e a t e d t o t h e d e s i r e d r u n t e m p e r a t u r e a f t e r takfing room c o n d i t i o n measurements. The a i r b a t h t e m p e r a t u r e I?eached t h e d e s i r e d t e s t t e m p e r a t u r e ~ J I i i n a b o u t 1-1/2 h o u r s , b u t a t l e a s t a n o t h e r f o u r h o u r s were J r e q u i r e d f o r t h e r o c k specimen t o r e a c h t h e t e s t t e m p e r a t u r e . During t e m p e r a t u r e changes t h e c o n f i n i n g f l u i d underwent d t h e r m a l e x p a n s i o n or contr3act i o n d e p e n d i n g upon whether h e a t i g J or c o o l i n g . l Repeated manual a d j u s t m e n t s were made t o keep t h e overburden pressure within t h e d e s i r e d l e v e l . When e q u i l i b r i u m t e m p e r a t u r e was r e a c h e d , f l u i d flow 4 w a s s t a r t e d and c o n t i n u e d f o r a b o u t a n h o u r b e f o r e measurements w e r e t a k e n . I R e p e a t e d measurement:s of t e m p e r a t u r e , p r e s s u r e s and I I flow r a t e w e r e made a t r e g u l a r t i m e i n t e r v a l s . Steady state w a s assumed when no change w a s o b s e r v e d i n t h e r e a d i n g s and ~ t h e s t e a d y v a l u e s were r e c o r d e d . A l l f l o w r a t e measurements were t a k e n a t room conditi.ons. 5.3 Measurements and C a l ~ c u l a t i o n s 5.3- 1 L i q u i d Flow: Three k i n d s o f l i q u i d s were used i n t h i s w o r k : d i s t i l l e d w a t e r , m i n e r a l o i l , and a l c o h o l . Tap w a t e r w a s d i s t i l l e d i n a B a r n s t e a d s t a i n l e s s s t e e l still. The o i l used w a s Chevron White M i n e r a l O i l No. 3 , ! I i I I and w a s c o m m e r c i a l l y a v a i l a b l e . - 2 8- The p h y s i c a l p r o p e r t i e s of 1 t h e o i l v a r i e d s l i g h t l y from one c o n t a i n e r t o a n o t h e r . a l c o h o l used w a s 2 - o c t a n o l ( P r a c t i c a l ) . The Before u s e , each l i q u i d w a s d e a e r a t e d u n d e r a vacuum of a b o u t 0.3 p s i a and f i It e r e d . To keep t h e f l u i d i n t h e l i q u i d s t a t e a t h i g h t e m p e r a + t u r e s , t h e e x i t f l o w i n g p r e s s u r e was k e p t c o n s t a n t at 2 0 0 p s i f o r a l l runs. An a c c u m u l a t o r , c h a r g e d t o 200 p s i , h e l p e p dampen pump p r e s s u r e p u l s a t i o n s and a l s o h e l p e d t o keep t h e f l o w i n g p r e s s u r e from c h a n g i n g d r a s t i c a l l y when t h e flow w a g s t a r t e d or s t o p p e d . Darcy's l a w f o r v i s c o u s f l o w i n a h o r i z o n t a l and l i n e a r I I p o r o u s medium i s : iI where q i s i n c c / s e c , k i s i n d a r c i e s , 1.1 i n c p , A i s i n c m2 and li i n atdcm. Eq. 5- 1 c a n b e e x p r e s s e d as: k = - 14700 -aLvw PAP where k i s i n m d , Ap i s i n p s i , w i n gm/sec, p i n gm/cc, a n d !I t h e o t h e r u n i t s and symbols a r e as d e f i n e d p r e v i o u s l y . Thia e q u a t i o n was used i n all c a l c u l a t i o n s . I n a d d i t i o n t o u s i n g Q e f s . 5 and 6 t o estimate t h e r e g i o n of v i s c o u s flow w l h e r e p o s s i b l e , c o n d i t i o n s o f viscousl , ~ f l o w were a l s o d e t e r m i n e d by o b t a i n i n g d a t a a t s e v e r a l f l o w r a t e s a t each t e m p e r a t u r e l e v e l and g r a p h i n g f l o w r a t e , q, - 2 9- versus pressure drop, p. F o r c o n d i t i o n s of v i s c o u s flow, t h e d a t a should f a l l on a s t r a i g h t l i n e , p a s s i n g t h r o u g h t h e origin. The o n s e t of non--Darcy f l o w was i n d i c a t e d by a down- ward c u r v a t u r e of t h e p l o t t e d p o i n t s f r o m t h e s t r a i g h t l i n e . I t i s n e c e s s a r y t o know t h e v i s c o s i t y and d e n s i t y of e a c h l i q u i d a t each working t e m p e r a t u r e l e v e l . Water d e n s i t y and v i s c o s i t y v e r s u s t e m p e r a t u r e were found i n t h e Steam T a b l e s z 3 and are p r e s e n t e d i n F i g s . 5 and 6 , and i n T a b l e 1, ' i 1 Appendix 9 . 1 . A c a p i l l a r y t u b e v i s c o m e t e r w a s c o n s t r u c t e d t o measure o i l and a l c o h o l (2-octanol.) v i s c o s i t i e s v e r s u s t e m p e r a t u r e a t t h e working p r e s s u r e l e v e l of 200 p s i . 11 The p r o c e d u r e f o r t h e s e measurements i s p r e s , e n t e d i n d e t a i l i n Appendix 9.3. The r e s u l t s of t h e s e measurements checked v e r y c l o s e l y w i t h I! t h e d a t a s u p p l i e d by t h e m a n u f a c t u r e r s and t h o s e found i n Iief. 39. The d e n s i t y of a l c o h o l a t v a r i o u s t e m p e r a t u r e s w a s measured w i t h a Bingham t y p e pycnometer. The d e n s i t y o f t h e o i l was measured a t 6OoF and t h e t a b l e s i n R e f . 2 4 were u s e d t o estimate t h e d e n s i t i e s a t h i g h e r t e m p e r a t u r e s . Results a r e shown i n F i g s . 7 t h r o u g h 1 0 , and T a b l e s 3 t h r o u g h 5 i n Appendix 9 . 1 . -30- '1 ~ , I 0 In M c. 0 0 M 0 Ln N 0 0 cv 0 Ln 4 0 0 d 0 Ln 0 0 0 0 t n !n 0 00 -31- 0 - 00 0 110 019 0,8 017 016 0 5 0 4 013 01 2 011 60 I 100 I I I 150 200 TEMPERATURE, 250 O F '=i~. F. !!ater lliscosityvs. TemDerature a t 290 n s i g -32- ?do I O185 \ OI84 0183 0 O182 \ 0 O1 81 \ 0 0.80 o179 OI78 100 Fig. 7. 150 200 250 300 lEMPERATURE, O F 9ensityvs.Temperature for Chevron White O i l ‘*e. 3 -33- a II- a a a c3 a w n 5- - w cn L 2 0 Q: zI V w v) 0 u 0 ' 0 v) W > 0 0 0 L n r f M o N m 4 omx)I\co 4 S3XOlS IlN33 F ~ F .8 . m a- M 6.k All S O X I r\ 3 I l V W 3 N I ] Viscosity v s . Temperature for Chevron White O i l No. 3 -34- c \0 \0 \0 \ 0 '\ 0 50 100 200 TEMPERATURE, 150 250 O F Fip. 9 . q e n s i t y of 2-nctanol v s . TemDerature a t 1 4 . 7 psi. -35- 300 10 9 8 7 6 5 4 3 0 \ 2 0 5 04 I I 4 I I 1 I 50 Fi.p. 10. 100 150 200 TEMPERATURE, 250 300 I O F l ’ i s c o s i t v o f 2 - k t a n o l vs. T e m e r a t u r e at 14.7 n s i -36- i 5.3-2 Gas Flow: Gas w a s s u p p l i e d f r o m h i g h p r e s s u r e c y l i n d e r s , and f l o w r a t e c o u l d b e r e g u l a t e d u p s t r e a m o f t h e c o r e by a t w o - s t a g e a d j u s t a b l e r e g u l a t o r equipped w i t h a r e - l i e f v a l v e , and downstretsm. hy means o f a n e e d l e v a l v e . Most experiments involved larrhar flow i n o r d e r t o o b t a i n a b s o l u t e p e r m e a b i l i t y and t h e Kliiikenberg s l i p f a c t o r . One v i s c o - i n e r t i a l r u n w a s made. I I n a d d i t i o n t o measuring p r e s s u r e d r o p , Ap, a s e p a r a t e I I t r a n s d u c e r w a s used t o measure t h e u p s t r e a m p r e s s u r e , p l . From t h e s e v a l u e s , t h e mean p r e s s u r e pm = p1 - I 1 AP 7 was corn- p u t e d , and t h e d i f f e r e n c e (p12-p22) w a s c a l c u l a t e d as 2pmAp. Low flow r a t e s w e r e measured w i t h a b u b b l e f i l m t y p e flowmeter and a Wet T e s t Yeter w a s used f o r h i g h flow r a t e measurements. Atmospheric p r e s s u r e and room t e m p e r a t u r e were a l s o r e c o r d e d t o pe:rmit c o r r e c t i o n s t o f l o w i n g c o n d i I tions. The i n t e g r a t e d f o r m o f Darcy's l a w which d e s c r i b e d s t e a d y h o r i z o n t a l l i n e a r g a s flow under i s o t h e r m a l c o n d i t i o n $ I is: where : = g a s f l o w r a t e a t room c o n d i t i o n s , cc/sec 9, k = absolute permeability, darcies A = c r o s s s e c t i o n a l area of porous medium, c m L = l e n g t h of p o r o u s medium, c m Ta = room t e m p e r a t u r e , OK -37- 2 T = f l o w i n g t e m p e r a t u r e , OK P a = room p r e s s u r e , a t m . a b s . Ap = p r e s s u r e d r o p across porous Fedium, atrr.. pm = mean p r e s s u r e w i t h i n porous medium, a t r . abs. v -z I = g a s v i s c o s i t y a t T and pm, c p = mean g a s c o m p r e s s i b i l i t y f a c t o r N i t r o g e n w a s t r e a t e d as a n i d e a l g a s and b e c a u s e of t h e l o w working p r e s s u r e r a n g e . t a k e n as 1 The r i g h t hand s i d e of Eq. 5-3 w a s d i v i d e d by 1 4 , 7 0 0 b e c a u s e , i n t h e l a b o r a t o r y , p r e s s u r e s were measured i n p s i and p e r m e a b i l i t i e s lated i n millidarcies. Thus: k, md =: 14,700 " 7 calc - -L1J.QaPaT AAPPmTa Gas v i s c o s i t y v e r s u s t e m p e r a t u r e i s g i v e n by S u t h e r l a n Q ' s 25 formula . For n i t r o g e n , N2: VN2 where T i s i n 0K - -1.3.85(10 -4 I T1 . 5 102+T and V is i n cp. Nitrogen v i s c o s i t y versus , I t e m p e r a t u r e a t atm0spheri.c p r e s s u r e i s p r e s e n t e d on F i g . 11 1 and i n T a b l e 2, Appendix 9 . 1 . No s i g n i f i c a n t i n c r e a s e i n n i t r o g e n v i s c o s i t y o c c u r s from a t m o s p h e r i c p r e s s u r e t o t h e I o p e r a t i n g l e v e l s , 2 0 0 p s i . , used i n t h i s s t u d y . E q s . 5-4 and 5-6 were used i n g a s f l o w c a l c u l a t i o n s I I I for v i s c o u s f l o w . See Appendices, s e c t i o n 9.3-2, -38- f o r analysis 0 0 M 0 Ln cu 0 0 (v 0 I n 4 0 Ln Lo cv - - CN 0 0 CN 0 0 0 N 00 0 0 0 0 - d 3 ‘AlIS03SII\ - 39- t-l - CD 4 - 0 0 of v i s c o - i n e r t i a l flow. A l i n e a r g r a p h of (p12-p22), ( p s i a )2 , where p1 i s upstream p r e s s u r e ( p s i a ) , p2 i s downstream p r e s s u r e ( p s i a ) , v e r s u s g a s flow r a t e , g, ( c c / s e c ) , w a s used t o d e t e r m i n e c o n d i t i o n s for v i s c o u s flow. -40- 6. ANALYSIS O'F P,ESULTS AND DISCUSSION The f o l l o w i n g p r e s e n t s t h e r e s u l t s found f o r t h e e f f e c t of t e m p e r a t u r e l e v e l and c o n f i n i n g p r e s s u r e on s i n g l e * phase f l o w i n sandstones. C o n f i n i n g p r e s s u r e had t h e e f f e c t of r e d u c i n g t h e a b s o l u t e p e r m e a b i l i t y o f s a n d s t o n e s f o r a l l t y p e s of f l u i d s used. S l i p f a c t o r f o r g a s flow w a s found t o be t e m p e r a t u r e dependent as p r e d i c t e d by t h e o r y . A change ( d e c r e a s e ) i n a b s o l u t e p e r n e a b i l i t y w i t h t e m p e r a t u r e increasles w a s o b s e r v e d o n l y i n t h e case o f water flow. 6.1 Water Flow Both c o n s o l i d a t e d and u n c o n s o l i d a t e d s a n d s t o n e s were used i n t h i s study. 6.1- 1 C o n s o l i d a t e d S a n d s t o n e s : The f i r s t experiment was c a r r i e d o u t w i t h a core t h a t was h e a t e d t o 3OO0C for 3 h r s and allowed t o c o o l o v e r n i g h t b e f o r e use. sents the r e s u l t . F i g . 1 2 pre- The r o c k w a s f i r s t h e l d a t 1 0 0 0 p s i con- I f i n i n g p r e s s u r e , and t h e a b s o l u t e p e r m e a b i l i t y was r e c o r d e d w i t h t e m p e r a t u r e i n c r e a s i n g t o 30OoF. The r o c k was t h e n a l l o w e d t o cool t o room t e m p e r a t u r e . Confining p r e s s u r e w a s i n c r e a s e d t o 2 0 0 0 p s i and t h e p r o c e s s o f h e a t i n g and measurement r e p e a t e d . The core h o l d e r used i n t h e work re- p o r t e d h e r e i n i s ra.ted a t 5 0 0 0 p s i a t 35OoF s a f e l y , b u t a maxinum of 4 0 0 0 p s i and 3OO0F w a s u s e d . -41- , I 0 Ln M ! 0 0 M 0 i I\ O Ln 4 0 0 0 4 0 . I I 0 0 Ln 0 0 a- I 1 0 0 0 0 M -42- cv 0 m 0 0 1 ; ~ ~ ~~ ~ ~~ I t c a n be s e e n from t h e graph t h a t a t e a c h l e v e l o f c o n f i n i n g p r e s s u r e , t h e a b s o l u t e p e r m e a b i l i t y t o water dec r e a s e d a t a n a p p r o x i m a t e r a t e of - 1.0 nd/OF. The n e x t s e r i e s of e x p e r i m e n t s w e r e performed on cores f i r e d a t 5OO0C i n o r d e r to i n v e s t i g a t e h y s t e r e s i s and r e p r o d u c i b i l i t y of r e s u l t s . 1 4 , and 1 5 . The r e s u l t s a r e shown on F i g s . 1 3 , A l l showed a d e c r e a s e of a b s o l u t e p e r m e a b i l i t y t o water w i t h t e m p e r a t u r e i n c r e a s e , b u t t h e s l o p e d e c r e a s e d with i n c r e a s i n g temperature. t o - 1.6 & / O F c w a s observed. An a v e r a g e s l o p e of - 1 . 3 rnd/OF The r e s u l t s a l s o show t h a t t h e t e m p e r a t u r e e f f e c t w a s e s s e n t i a l l y r e v e r s i b l e (see F i g . 1 3 ) . The f i r s t c o o l i n g c y c l e f o r t h e M a s s i l l o n S a n d s t o n e Nol 3 ( F i g . 14) a t 3 0 0 0 p s i g c o n f i n i n g p r e s s u r e i n d i c a t e d h y s t e r d - .. sis. On t h e f i r s t c o o l i n g c y c l e , t h e pern-!eability with respect t o the f i r s t : heating cycle. increased ~ On h e a t i n g and cool/ing a g a i n , r e s u l t s f o l l o w e d t:he f i r s t c o o l i n g r u n , i n d i c a t i n g telrp e r a t u r e r e v e r s i b i l i t y arid good r e p r o d u c i b i l i t y . No r e a s o n for t h e i n c r e a s e i n p e r m a b i l i t y after t h e first h e a t i n g r u n I w a s found. 6.1-2 U n c o n s o l i d a t e d Sand: The f i r s t e x p e r i m e n t i n t h q s s e r i e s w a s r u n w i t h u n c o n s o l i d a t e d O t t a w a S i l i c a Sand of a v e r a g e g r a i n s i z e of 0 . 3 8 5 mm, T h i s core w a s n o t s u b j e c t e d t o h e a t t r e a t m e n t and was l o a d e d as o u t l i n e d i n t h e p r o c e d u r s e c t i o n 5. , ~ 3, Data were not: o b t a i n e d f o r t h e c o o l i n g c y c l e s . The r e s u l t s a r e shown i n F i g . 1 6 . 1 0 0 0 , and 1500 p s i g were u s e d . C o n f i n i n g p r e s s u r e s o f 500i, A b s o l u t e p e r m e a b i l i t y t o watw 1 - 43- I, -44- 0 I n M 0 0 M 0 J m cv J 0 0 cv 0 m 4 3 0 0 3 4 4 0 0 0 Ln 0 0 M 0 0 cv LA 0 0 I U - c3 U v) Q 0 0 0 M II - v) cn w (1: Q c3 z z H I L z 0 V I I 0 0 4- 1 0 0 M -45- I 0 0 cv 0 0 -I 0 In M 0 0 M 0 Gi c ( In cv v) CL 0 0 cv II 0 0 cv z 4 E 0 In 4 h ic, 0 0 4 ’. M I 1 I I I 0 0 0 0 0 0 0 0 0 u3 Ln a- ‘A11 1I IfW3Wt13d -46- M 0 w 4rl 0 Ln 0 0 4 4 0 In M v) n m O 0 00 M 0 0 - c v o II M II 0 Ln cv E W t r r e o n n - Z a z v ) 0 0 cv 0 In l l 0 0 1 1 0 0 0 % cv N 0 c3 0 0 0 0 00'1 1 a- % l l 0 Ln 0 0 0 % 0 1 -47- 0 0 0 0 0 decreased w i t h an increase i n confining pressure. "he r a t e of c h a n g e was - 0 . 5 rnd/OF a t a11 l e v e l s of c o n f i n i n g p r e s s u r e c As t h e a b s o l u t e p e r m e a b i l i t y of t h i s core w a s v e r y h i g h , (1 2 2 , 0 0 0 md a t 500 p s i g c o : n f i n i n g p r e s s u r e , t h e a v e r a g e s a n d g r a i n s i z e was r e d u c e d for t h e n e x t e x p e r i m e n t . 1 See Ref. 26 1 f o r methods of c o n t r o l o f p e r m e a b i l i t y and p o r o s i t y of synt h e t i c sands. 6.2 1 Gas F l o w Gas f l o w e x p e r i m e n t s were c o n d u c t e d a t t h r e e d i f f e r e n t t e m p e r a t u r e l e v e l s and a r a n g e of c o n f i n i n g p r e s s u r e s . 1 1 Abso- l u t e p e r m e a b i l i t i e s were measured w i t h n i t r o g e n flow under c o n d i t i o n s of v i s c o u s flow and g r a p h e d as a f u n c t i o n of t h e r e c i p r o c a l mean p r e s s u r e on a c o n v e n t i o n a l K l i n k e n b e r g graph. One r u n w a s conducted i n t h e v i s c o - i n e r t i a l flow r e g i o n for a consolidated sandstone. D e t a i l s of t h e a n a l y s i s of t h i s I 1 1 1 g a s flow d a t a are g i v e n i n T a b l e 9 and i n Appendix ( s e c t i o n 9.3- 2). I n a l l cases, t h e absolute permeabilities at d i f f e r e a t t e m p e r a t u r e s b u t for t h e same c o n f i n i n g p r e s s u r e , e x t r a p o l a t e d t o t h e same i n f i n i t e p r e s s u r e v a l u e . The s l o p e s o f t h e s e ! g r a p h s are, however, p r o b a b l y n o t t r u e K l i n k e n b e r g s l i p c o e f ficients. I The h i g h s l o p e s a r e a r e s u l t of t h e e f f e c t s of a i c o m b i n a t i o n of b o t h s l i p and mean p o r e p r e s s u r e - c o n f i n i n g p r e s *I I s u r e stress e f f e c t s on p e r m e a b i l i t y . Although t h e c o n f i n i n g p r e s s u r e was h e l d c o n s t a n t a t 1000. psi o r more, t h e p o r e p r e s s u r e changed from n e a r l y a t m o s p h e r i c t o s e v e r a l hundred p s i for e a c h s e r i e s of r u n s . 3 e t e r m i n a t i o n of s l i p c o e f f i c i e n t s w a s n o t a m a j o r o b j e c t i v e of t h i s s t u d y . 'I The v a l u a b l e informadl t i o n from t h e s e graphs is t h a t t e m p e r a t u r e has no a p p a r e n t effect o n a b s o l u t e p e r m e a b i l i t y t o gas. -49- 0 L n M 0 0 M 0 Ln cv 0 0 N 0 Ln 4 8 0 4 0 I n 0 0 r3 0 3 CD -49- 6.2-1 Consolidatetl Sandstones: The r e s u l t s of t h e f i r s t r u n i n t h e v i s c o u s and v i s c o - i n e r t i a l f l o w r e g i o n s on M a s s i l l o n C o n s o l i d a t e d Sandstone Core Yo. 5 are shown on F i g s . 18 and 19, r e s p e c t i v e l y . On Fig. 1 8 , t h e Klinkenberg s l i p f a c t o r s a t 6 8 , 1 5 0 , and 25OoF a r e 2 . 2 6 4 , psi, respectively. I 3.587, and 4.351 This shows t h a t t h e a p p a r e n t Klinkenberg s l i p f a c t o r depends upon t e m p e r a t u r e . T h e a p p a r e n t permea- I b i l i t i e s a t d i f f e r e n t t e m p e r a t u r e s and p r e s s u r e s e x t r a p o l a t e d t o t h e same v a l u e o f 9 6 0 md and a g r e e r e a s o n a b l y w i t h t h e v i s c i n e r t i a l a n a l y s i s v a l u e o f 9 3 2 md shown on F i g . 1 9 . The t u r b u d l e n c e f a c t o r 8 , which may be o b t a i n e d from F i g . 1 9 , was 1 . 7 x 7 10 f t - l , and i s i n agree,ment w i t h a c o r r e l a t i o n proposed i n Ref. 27. 1 The c o n f i n i n g p r e s s u r e was h e l d c o n s t a n t a t 1 0 0 0 p s i i n these runs. Another s e r i e s o f experiments w a s conducted on Massillon Sandstone Core N o . 6 a t room, 15OoF, and 25OoF t e m p e r a t u r e i !I l e v e l s and a t c o n f i n i n g p r e s s u r e s of L O O O , 3000, and 4000 p s i g . ! R e s u l t s are shown on F i g s , , 2 0 - 2 2 , and a r e similar t o t h o s e of 11 Fig. 18. 1, 1 Absolute permeability decreased w i t h an i n c r e a s e i n c o n f i n i n g p r e s s u r e ; and at: t h e same l e v e l of c o n f i n i n g p r e s s u r q I t h e a p p a r e n t p e r m e a b i l i t i e s e x t r a p o l a t e d t o t h e same i n f i n i t e p r e s s u r e v a l u e a p p a r e n t s l i p f a c t o r s a t room and 15OoF tempera-i t u r e l e v e l s w e r e e s s e n t i a l l y t h e same for a l l l e v e l s o f conf i n i n g p r e s s u r e , b u t h i g h e r a t 2 5OoF t e m p e r a t u r e . The v a l u e s o f a b s o l u t e p e r m e a b i l i t i e s o b t a i n e d w i t h ni.trop,cn flow a n d wstcr flow for t h c c o n s o l i d c i t e d s a n d s t o n e cores w e r e different. I I I P e r m e a b i l i t i e s t o water a t room t e m ~ perature ranged between 550 rrd and 4 5 0 md f o r a l l of t h e -50- u, 0 0 Ln N II I- L L L L 0 0 0 0 0 L n c D I+ II II I- t- \ U v) a 0 0 0 4 II w p: 3 v) v) w p: n (3 z z U U L z 0 u 0 0 (7W 0 0 cn ‘AlIlI€fW3W~3dlN3tlWddb -51- 1.4 1.2 n cv I I- 1.0 LL v '0 4 0.8 0.6 0,4 0.2 , 0 -57- L - %I 3 LI 0 0 Ln cv 3 n - 4 0 ca I 0 Ln E a 3 W E 3 - Ef u 0 @a, P'SI 0 *o - M 0 a 0 0 E a w u w cr: 0 0 m -53- Q 0 co 0 0 h d - co 0 J J u0 0 Lo 0 t-I .J J J J 4 d CI] J 0 0 0 -I 0 0 cn 0 0 00 J -54- - w LT 3 t- a LT w a LL 0 0 Ln 5 I- L L L L L L 0 0 0 0 0 0 r \ m m d c v 0 . 0 1 L L 0 C 3 Ln CV 0 0 m I\ 0 aW 'AlIlI8V3Wkl3d -55- 0 lN3klVddv J confining p r e s s u r e l e v e l s , while absolute p e r m e a b i l i t i e s t o n i t r o g e n were c o n s i d e r a b l l y h i g h e r and r a n g e d from 9 6 0 md t o 800 md f o r t h e same c o n d i t i o n s . T h i s s u g g e s t s t h a t t h e phen- d omena c a u s i n g t h e p e r m e a . b i l i t y r e d u c t i o n w i t h w a t e r f l o w a t room t e m p e r a t u r e may also be r e s p o n s i b l e for t h e p e r m e a b i l i t y reduction a t high temperatures. The M a s s i l l o n S a n d s t o n e has a low c l a y c o n t e n t , a n d had been f i r e d at 50OoC. 6.2- 2 U n c o n s o l i d a t e d Sand: F i g . tained with f i r e d s i l i c a sand. 4 i 23 shows r e s u l t s ob- A 2000 p s i g c o n f i n i n g p r e s s u ri e J w a s a p p l i e d , and t h e t e m p e r a t u r e l e v e l s used were 68OF, 150af, and 25OoF. The r e s u l t s were s i m i l a r t o t h o s e for t h e consol,!- dated sandstones. 4 I P e r m e a b i l i t y t o w a t e r w a s a l s o measured f o r t h i s core.' While t h e e x t r a p o l a t e d a b s o l u t e p e r r e a b i l i t y t o n i t r o g e n w a s / 4,260 md, t h e p e r m e a b i l i t y t o water was o n l y 2 , 1 2 7 md a t r o q temperature. 6.3 1" J O i l Flow ~ .J Because of t h e d i f f e r e n c e between t h e r e s u l t s o b t a i n e d ~ a t e l e v a t e d t e m p e r a t u r e s w i t h water f l o w and g a s f l o w , s i m i l g r experiments w e r e r u n w i t h another f l u i d . Chevron White O i l ~ J No. 3 w a s c h o s e n for i t s h i g h e r v i s c o s i t y and i t s n o n - p o l a r j characteristics as opposed t o w a t e r , which i s a n i n t e r m e d i d t e v i s c o s i t y p o l a r f l u i d a n d may i n t e r a c t w i t h t h e r o c k s u r f a c e l d Experiments (see 3.ef. 1) had a l r e a d y been c a r r i e d o u t w i t h Chevron White O i l No. 1 5 , which i s v e r y v i s c o u s . A s i n water I f l o w or g a s f l o w e x p e r i m e n t s , t h e combined e f f e c t of temperait I t u r e and o v e r b u r d e n p r e s s u r e was i n v e s t i g a t e d . -56- ~ 4 11 -t I- a 0 0 J 3 I n 0 0 0 3 Ln 0 0 co a3 -57- 0 0 Lo -3 0 0 0 N 3 a- J F i g s . 2 4 and 25 show t h e r e s u l t s w i t h o i l f l o w for c o r e s No. 1 0 and 11. solidated sandstones. O i l flow w a s cofiducted o n l y on con- Absolute permeability t o o i l w a s J a f f e c t e d by c o n f i n i n g p r e s s u r e , as e x p e c t e d , b u t t h e r e w a s only a s l i g h t decrease i n a b s o l u t e permeability t o o i l w i t h temperature increase. Hysteresis effects i n cooling cycles J were more pronounced a t h i g h c o n f i n i n g p r e s s u r e s o f 3 0 0 0 p s i and 4 0 0 0 p s i . J P e r m e a b i l i t y l e v e l s a t room t e m p e r a t u r e a g r e e c l o s e l y 1 I with t h o s e o b t a i n e d w i t h n i t r o g e n flow. T h e a b s e n c e of r o c k - o i l i n t e r a c t i o n i s b e l i e v e d t o b e r e s p o n s i b l e for the i I d i f f e r e n c e between water and o i l p e r m e a b i l i t i e s . T h i s sug- 1 g e s t s a d e f i n i t e i n t e r a c t i o n between water and s a n d s t o n e , I consolidated or unconsolidated. I 6.4 J i) I 2- Octanol Flow I n view of t h e r e s u l t s w i t h water, it a p p e a r e d u s e f u l t o run s i m i l a r e x p e r i m e n t s w i t h a n o t h e r polar l i q u i d . .J 2- octanol a l c o h o l w a s chosen. E x p e r i m e n t s were c o n d u c t e d w i t h commercial g r a d e 2o c t a n o l , and t h e r e s u l t s a r e p r e s e n t e d i n F i g . 2 6 . The un4 c o n s o l i d a t e d O t t a w a S i l i c a Sandcore used was f i r e d a t 50OoC. I I The a v e r a g e s a n d g r a i n s i z e w a s 0 . 1 5 6 mm. The c o n f i n i n g p r e s s u r e a f f e c t e d t h e a b s o l u t e p e r m e a b i l i t y as e x p e c t e d , b u t i ~ -4 t e m p e r a t u r e a p p e a r e d t o c a u s e a. small i n c r e a s e i n a b s o l u t e permeability. I n a d d i t i o n , t h e r e w a s a permanent r e d u c t i o n I i n absolute p e r n e a b i l i t y on each cooling cycle. These r e s u l d s J a r e d r a m a t i c when compared t o t h e water d a t a on F i g s . 1 6 and,117. -58. l 0 0 M n 0 O I n N GO 0 Ln 0 4 0 0 4 0 d 0 Ln 0 0 m 0 0 00 0 0 0 0 to 0 0 Ln J rl rl z0 J c ( cn a a 0 0 0 cv J 0 M J 0 m cv i z i a W r LL 0 J J 0 I n 4 0 0 J J 4 J I Q 0 0 4 I I I I 0 0 00 0 0 R 0 0 Lo 0 0 0 i n 4 J aW ' A l I l I 8 V 3 W W d -60J v) v) o w “CY w a a (3 O Z 0O Z 4“ - 0 0 N 0 II II v) N - w v) & W v) E Q, z W a U CY 0 c3 a, z a = w l a 0 a e c1 z a cn 0 0 I n 4 \ 0 0 d 0 0 0 e I I 0 0 0 0 0 0 0 -l T 0 0 -l 0 4 cn I 00 -61- I l 0 3 0 0 0 0 -l % r\ Lo 0 0 0 0 % I n Ln - I I , The s l i g h t i n c r e a s e i n p e r m e a b i l i t y t o o c t a n o l w i t h temperat u r e i n c r e a s e f o r b o t h h e a t i n g and c o o l i n g r u n s emphasizes t h e i m p o r t a n c e of t h e d e c r e a s e i n k w i t h t e m p e r a t u r e i n c r e a s e for water. 3 R e c e n t d i s c u s s i o n s between Ramey and Dreher (Yara- thon O i l Co., Denver) r e v e a l e d t h a t o c t a n o l o f t e n behaves more l i k e an o i l t h a n a n aqueous w e t t i n g p h a s e i n s a n d s t o n e s . In d r e t r o s p e c t , it might have been b e t t e r t o h a v e s e l e c t e d b o p r o p y l a l c o h o l (IPA) as t h e second p o l a r s u b s t a n c e . It i s recommended t h a t I P A be c o n s i d e r e d f o r f u t u r e s t u d i e s . 6.5 J Discussion Cass6’ c o n c l u d e d t h a t c l a y - w a t e r i n t e r a c t i o n s may I h a v e b e e n o n e r e a s o n for t l h e e f f e c t o f t e m p e r a t u r e l e v e l upon 1I J i a b s o l u t e p e r m e a b i l i t y t o w a t e r f o r sandstones h e observed. I ~ Grim3’ 31 p r e s e n t e d a comprehensive r e v i e w of t h e m e c h a n i s m involved i n clay- water i n t e r a c t i o n s . J Because t h e r o c k s u s e d i n t h i s work w e r e t o t a l l y or n e a r l y c l a y - f r e e , c l a y - w a t e r ~ i n t e r a c t i o n i s c o n s i d e r e d r e s p o n s i b l e f o r o n l y a minor role 1 .d i n t h e phenomenon o b s e r v e d i n t h i s s t u d y . I t i s almost c e r t a i n t h a t water- cilica i n t e r a c t i o n s a r e r e s p o n s i b l e f o r t h e mafior e f f e c t s o b s e r v e d w i t h w a t e r . In! 3 a d d i t i o n t o t h e r e s u l t s of t h i s s t u d y , G r u n b e r g and N i s s a n 13 I rrd a t room t e m p e r a t u r e ) ’I \ u s e d a q u e o u s s o l u t i o n s ( i n c l u d i n g Amyl Alcohol) w i t h J e n a Glass F i l t e r s of low p e r m e a b i l i t y ( 1 6 0 and found a l i n e a r d e c r e a s e i n a b s o l u t e p e r n e a b i l i t y w i t h a n 1 J increase i n temperature. F l u i d f l o w mechanisms 32 often fit t w o c a t e g o r i e s : 3 (1) mechanisms which a r e e s s e n t i a l l y m e c h a n i c a l i n n a t u r e , t h e -62- 1 1 f l o w d e p e n d i n g on t h e b u l k p r o p e r t i e s of t h e f l u i d s c o n c e r n e d and upon the m e c h a n i c a l f o r c e s e x e r t e d upon t h e f l u i d b o d i e s ; mechanisms which a r e e s s e n t i a l l y m o l e c u l a r i n char&- and ( 2 t e r , t h e f l o w d e p e n d i n g l a r g e l y o n t h e motion of t h e i n d i v i d u a l m o l e c u l e s , t h e moleculair, w e i g h t , t h e c o l l i s i o n cross- section, t h e mean f r e e p a t h , r o c k - f l u i d a t t r a c t i v e f o r c e s , e t c . , r a t d e r t h a n upon t h e d e n s i t y , p r e s s u r e v i s c o s i t y , e t c . , of t h e f l u i d i n bulk. The l a t t e r mechanisms may be d o m i n a n t i n t h e case of t h e e f f e c t of t e m p e r a t u r e upon w a t e r f l o w i n s a n d s t o n e s under p r e s s u r e . S u r f a c e a t t r a c t i v e forces between s i l i c a and w a t e r m o l e c u l e s may be l a r g e enough t o l e a d t o c h e m i - s o r p t i o n . In s u c h a case, t h e a d s o r b a t e m o l e c u l e s become p r a c t i c a l l y a p a r t o f t h e solid s u r f a c e a n d , compared with o t h e r rnolecules .. i n t h e l i q u i d , s u c h chemfi-sorbed m o l e c u l e s may be l a r g e l y immobilized. The e f f e c t i v e c r o s s - s e c t i o n u n d e r v i s c o u s f l o w I c o u l d t h e n b e d i f f e r e n t f o r water from t h e o t h e r f l u i d s t e s t & . I n c r e a s e s i n t e m p e r a t ~ r eseem ~ ~ t o i n c r e a s e t h i s e f f e c t from t h e r e s u l t s of t h i s s t u d y . An e x h a u s t i v e l i t e r a t u r e s u r v e y i n d i c a t e d n o known p h e n o m n a c a p a b l e of e x p l a i n i n g t h e magnit u d e of t h e e f f e c t s o b s e r v e d i n t h i s s t u d y . It is b e l i e v e d t h a t a major, a n d h e r e t o f o r e u n s u s p e c t e d a t t r a c t i o n between water and s i l i c a h a s been d i s c o v e r e d . It is p o s s i b l e t h a t t h i s a t t r a c t i o n i s e s s e n t i a l l y r e s p o n s i b l e for t h e l a r g e t e m p e r a t u r e e f f e c t s on p r a c t i c a l i r r e d u c i b l e water s a t u r a t i o n and r e l a t i v e p e r m e a b i l i t i e s 34916,35, and on c a p i l l a r y p r e s ! - s u r e s 36-38 and r e s i s t i v i t y p r e v i o u s l y r e p o r t e d . - 6 3- 1 J If a s t r o n g a t t r a c t i o n between water and s i l i c a i s _. t h e major t e m p e r a t u r e e f f e c t , s e v e r a l new e x p e r i m e n t s w i t h v, g a s - o i l flow i n s a n d s t o n e s w i l l show no t e m p e r a t u r e e f f e c t , I ~ w h i l e g a s - w a t e r f l o w i n s a n d s t o n e w i l l depend on t e m p e r a t u r e . I n a d d i t i o n , e x p e r i m e n t s of any s o r t i n l i m e s t o n e s s h o u l d J n o t depend s t r o n g l y on t e n p e r a t w e . i J d J J J J J -64J 7. C O N C L U S I 3 N S AND RECOY!!!TYIkTIONS E x p e r i m e n t a l r e s u l t s i n d i c a t e t h a t t h e a b s o l u t e perm e a b i l i t y t o water f o r c o n f i n e d s a n d s t o n e s i s s t r o n g l y t e m p e r a t u r e dependent. The a b s o l u t e p e r m e a b i l i t y of s a n d s t o n e s t o other f l u i d s (nitrogen, mineral o i l , octanol) i s e i t h e r , u n a f f e c t e d o r o n l y s l i g h t l y a f f e c t e d by t e m p e r a t u r e l e v e l . Temperature increase has t h e e f f e c t of d e c r e a s i n g t h e a b s o l u t e permeability t o w a t e r f o r sandstones remarkably. T e m p e r a t u r e c h a n g e h a s l i t t l e o r no e f f e c t on t h e abeol u t e p e r m e a b i l i t y o f s a n d s t o n e s t o n i t r o g e n , m i n e r a l oil, qr octanol. I n t h e case o f water flOt7, permeability reductiohs o f up t o 6 0 % were o b s e w e d o v e r a t e m p e r a t u r e r a n g e o f 70-$OO0F. ~ R e g a r d l e s s of t h e t y p e of f l o w i n g f l u i d , t h e l e v e l o f c o n f i n i n g p r e s s u r e a f f e c t e d a b s o l u t e p e r m e a b i l i t y i n t h e s@ne manner , i . e . , permeability d e c r e a s e d w i t h i n c r e a s i n g confizhing For water f:Low e x p e r i m e n t s , i n c r e a s i n g t h e c o n f i n i n g pressure. p r e s s u r e had t h e a d d i t i o n a l e f f e c t of i n t e n s i f y i n g t h e tembera- t u r e dependence o f a b s o l u t e p e r m e a b i l i t y i n many cases (but not a l l ) . I n t h e l i g h t o f t h e r e s u l t s o b t a i n e d , it seems t h a t wnsuspected f l u i d - s o l i d s u r f a c e a t t r a c t i v e f o r c e s between w a t e r , m o l e c u l e s and s i l i c a were l a r g e l y r e s p o n s i b l e for t h e m a j o r e f f e c t s observed. pertinent The f o l l o w i n g r e c o m n e n d a t i o n s a p p e a r . -65- -66- J' I t i s r e c o r n e n d e d t h a t t h e r e s u l t s o b t a i n e d by G r u n 13 b e r g and N i s s a n b e r e c h e c k e d for t h e same a a u e o u s s c l u t i o n s and for c o n f i n e d p o r o u s media. It i s also r e c o r n e n d e d t h a t J e x p e r i m e n t s b e r e p e a t e d f o r h i g h e r t e m p e r a t u r e s and c o n f i n i n , g pressures. S i n c e o c t a n o l behaves more l i k e a n o i l t h a n a n aq-ueous J w e t t i n g p h a s e i n s a n d s t o n e s , it i s recommended t h a t i s o p r o p y l alcohol b e used as t h e second polar s u b s t a n c e for f u t u r e studies. R e s u l t s from such s t u d i e s may h e l p t o e x p l a i n whether A t h e d e c r e a s e i n water p e r m e a b i l i t y w i t h i n c r e a s i n p t e m p e r a t q h e I is due t o t h e p o l a r i t y o f water. d I f a s t r o n g a t t r a c t i o n between w a t e r and s i l i c a c a u s e s ' t h e t e m p e r a t u r e e f f e c t , e x p e r i m e n t s d e s i g n e d t o i s o l a t e watap a n d / o r s i l i c a w i l l be e n l i g h t e n i n g . E x p e r i m e n t s w i t h water I f l o w i n l i m e s t o n e s s h o u l d n o t depend s t r o n F l y o n t e m p e r a t u r a I n a d d i t i o n , e x p e r i m e n t s w i t h g a s - o i l f l o w i n s a n d s t o n e s may show n o t e m p e r a t u r e e f f e c t w h i l e g a s - w a t e r f l o w i n s a n d s t o n d w i l l depend on t e m p e r a t u r e . J i J J -66- 8. 1. REFERENCES Cassg , F. J . : "The E f f e c t o f T e m p e r a t u r e and C o n f i n i n g P r e s s u r e on F l u i d Flow P r o p e r t i e s of C o n s o l i d a t e d Xocks ," Ph.D. D i s s e r t a t i o n , S t a n f o r d U n i v e r s i t y ( 1 9 7 4 ) . 2. A r i h a r a , N . : "A Stud17 of N o n - I s o t h e r m a l S i n g l e and TwoPhase Flow t h r o u g h C o n s o l i d a t e d S a n d s t o n e s ,!' Ph.D. D i s s e r t a t i o n , Stanford University (1974). 3. Greenberg, D . 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Mineralogy, M c G r a w - H i l l Book Book Company, - 34. P o s t o n , S . W . , Ysrael, S. , H o s s a i n , A.K.M.S. , Montgomery, E . F . , 111, and Rarney, H . F . , Jr.: "The E f f e c t o f Tempevat u r e on I r r e d u c i b l e Water S a t u r a t i o n and R e l a t i v e Permedb i l i t y of U n c o n s o l - i d a t e d Sands," SOC. of P e t . Eng. Joqr. (June 19701, 1 7 1 . 35. Weinbrandt, R.M., Casse, F , J . , and Ramey, H . J . , Jr.: "The E f f e c t o f T e m p e r a t u r e on R e l a t i v e and A b s o l u t e P e r m e a b i l i t y of S a n d s t o n e s , " SOC. of P e t . Eng. J o u r . ( O c t . 1 9 7 5 1 , 376. , ' 36. S i n n o k r o t , A.A. , Ramey, Hi; J . , Jr, , a n d Marsden, S.S ,, J r , : "Effect of T e m p e r a t u r e L e v e l upon C a p i l l a r y P r e s s u r e ' Curves," SOC. o f P e t . Eng. J o u r . (March 19711, 1 3 . 37. J r . , and Ramey, H.J., Jr. E Okandan, E . , Marsden, S .S., " C a p i l l a r y P r e s s u ~ eand C o n t a c t Angle Measurements at E l e v a t e d T e m p e r a t u r e s , I 1 p r e s e n t e d a t AIChE M e e t i n g , FLlsa, Oklahoma, March 1:2, 1 9 7 4 . 38. S a n y a l , S . K . , Ramey, H . J . , J r . , and Marsden, S . S . , Jri. : "The E f f e c t o f T e i n p e r a t u r e on C a p i l l a r y P r e s s u r e P r o p k r t i e s of Rocks," S:PWLA 1 4 t h Annual Logging Symposium (May 1 9 7 3 ) . 39. N a t i o n a l R e s e a r c h C o u n c i l o f U. S .A. : " I n t e r n a t i o n a l C r i t i c a l T a b l e s o f Numerical Data, P h y s i c s , C h e m i s t r y and Technology," 'Vol. I-1111, 1 9 3 3 , ~ -69- J 9. APPENDICES J 3 c 9.1 L:st of Tabulated ! l a t a J T a b l e 1. D e n s i t y and V i . s c o s i t y of Water v s . Temperature r' (from Steam Pressure = 200 p s i g J Temperature . ' Density gm/cc Viscosity 60 0.9990 1.100 100 0.9931 0.679 150 0.9803 0.426 200 0.9632 0.300 250 0.9423 0.228 300 0.9180 0.183 350 0.8904 0.152 OF cp J 4 J 4 4 3 4 -72- c T a b l e 2. V i s c o s i t y of N i t r o g e n vs. T e m p e r a t u r e I Pr-essure = 14.7 Temperature OF ' psia Temperature Viscosity cp OK 60 288.7 0.01739 100 310.9 0.01839 150 338.7 0.01959 200 366.5 0.02074 2 50 394.3 0.02185 300 422.0 0.02291 I OK -73- = T(°F)-32 1.8 + 273.16 J J J J si a 0 n f U 5 u 0 rl k Q, rl rl Ln F f m . co 0 0 0 0 0 0 m CD 03 03 3. 03 f rl 0 . 0 0 0 03 Lo CD m 0 3 (D Ln W a f * 0 0 rl J 9 0 0 0 0 J I E J W v) I 0 rl X b a VlD.413 0 0 0 0 0 0 J hl + ri U 0 t-i ri v) 3 0 II E b : . I J Q) c 3 -74J I cv $1 I cv ti N b4- 0 E: rd 0 I c 0, n +J a Llc4 -75- W O Table 5. Viscosity of 2-Octanol vs. T e m p e r a t u r e J Pressure = 200 psig I ! Temp. “T A P Q lJ cpTsec ps1-cc psi cc/sec 66 0.05112 1.50 0.00725 100 0.05117 1.25 0.01266 5.0 150 0.05124 1.00 0.02222 2.306 200 0.05131 1.00 0.04000 250 0.05138 0.75 0.04494 300 0.05144 OF + J .J 0.8 7 J where aT. = .05113 0.75 0.0625 0.6L4 1 + 2 . 6 7 ~ 1 0 - ~(T-7O0F‘I] 3 J -76- '1 It X E N I I I b2 G ' - E u .rl rnm acv Lm m o Q , C D o ~ m o C D o o o o c o o ~ m o u l o m m ~ c - ( V O ( V m ~ N O f c n ~ ~ 0 h l m 0 c v 0 c v ~ a , C D f m h l ~ c n f m c v d 0 7 ~ m ( V ~ ~ ~ m c v ~ o c v c o 0 . ' II II It ..................... h l m j O O O O O O O O O O O O Q O O O O O O O O 5d 5Q ) a < Q i r n E - l m $a Z& 2-g 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 000000000000000000000 000000000000000000000 r l ~ d ~ l d d ( V c v N ~ c v m 0 m m m ~ ~ ~ j f 3 Q) c 0 +J rn a c a fmac-cnmffbcnmdcvulm b m r ( c ' ~ o ~ ~ c o u 3 j a , o d o c - ~ c n j ~ m ~ o m ~ I ~ c n d c v c v r l c v d ( V c v ( V d ~ ~ ~ r l 0 c-mffcom ...................... 0000'0d000000000000000 000000000000000000000 v) c 0 rl Fc 0 44 a +J rd n 3 0 d Ll W Q) d A a b - 7 7- + -P c 0 V 4 J nib CD a303 o r l c n 0 . m II Q & 3 . m f II II ) J zl "I . . . . . . . . . . . . . . . . . . . . . . . . . 0 0 0 0 CI 0 0 0 0 0 0 0 0 0 0 d rl 0 0 0 0 0 0 0 0 < 0000000000000000000000000 [I] v) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 c> 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 E l - i l - i l - i r l r i r l l - i ~ ~ m ~ ~ ~ v ~ ~ ~ ~ m o m m o m m o ~ P-! J A. Q[I] 0 0 0 0 ~ 0 ~ 0 ~ f r l r l l - i f ~ 0 0 f W f h l ~ f O ~ .......................... ~ O N ~ ~ I m f ~ ~ N ~ N N ~ m ~ m m W h l W N 0000000000000000000000000 W,l P O - ~ 0 0 0 0 0 ~ b m 0 LD 0 m rr(mmCvr4 J m 0 0 0 0 0 0 0m l-immmhlhlrl UJ0 Ln 0 UJ 0 0 0 0 0 0 0 0 u3 u3 UJ 0 Lo 0 Ln 0 In d N m m m h l d 0 + 0 0 3 J W 31n X ; 1 m 0 I-4 I1 x co CD co 0 aJ CI) CD 0 0 CD 0 OD 0 03 0 a 0 0 hl N N a3 N CI) N u3 CD N 0 N OD N 0 01 0 d f zt N r l w m f c n m f m d~ h l m f m 0 .................. I-4 0 0 0 0 0 c> 0 0 0 0 0 0 0 0 0 0 0 c 000 0 0 0 0 0 00 000 00 0 0 0 m mmmm 0 m m a, o c> c> 0 0 0 0 0 0 0'0 000 0 0 0 0 000 00 0 0 0 00 0 0 000 0 0 0 0 cr) m m f f f f f f f f f CJ 0 r\l c> cu m 0 0 m N N 0 N hl mf o m o cr) rr) o co o o cr) m co m m o w mODC0 f 43 (D 00 0 Q, 00 j 1-43CD 03 CT, a, 0 0) a, 0 3 cn cn 0 0 , m a, 0, cn m Q, m o m .................. 0 0 0 0 0 0 (30 0 0 0 0 0 0 0 0 0 0 0 CD CD a3 0 co (9 b rn b ff 0, d Ln m m 6, b fi co 0 CD CD a3 m I+ l il-i d l id I-4 cu rl rl rl rt 0 0 0 0 0 0 (20 0 0 0 0 0 0 0 0 0 0 a, 0, co 0743 rl rl I-4 rl rl 4 b fr) cn co (3, .................. 0 0 0 0 0 0 (30 0 0 0 0 0 0 0 0 0 0 00 0 N 0 ru . j . 0 00 hl OD m N f hl mf 0 . .m. . . . . . .m. . . . . . . . . Lo m N hl 6JC-J m 3 04 c\1 CJ N 04 N mw 0 0 0 0 0 0 '3 0 0 00000 0 000 a 3c .?I u c 0 0 21 -79- m -I J m m f co m m b a, m 0 rl 0 r l f N 00 0 a, CD a, i-l LO i-l Lo 0 a, (v rl co r l c o CJ v) 0 b Lo m m 0 cv (v CJ m m m m m m hi N I 3 m m m 0 rl X 0 co 0 co m 00 0 co 0 0 co 0 co cr) OD 0 co Lo cv a0 cv 0 N c- m CJ 0 CJ OD N 0 hl m c n f mcu r l C J mrfcoa, f m h i r l N m f c n Lo CJO .................. 000 bl ( u a + J F c R l & 3 04 a m P a, " F c 3 0 & 0 0 Q\ tu c3 0 0 0 c3 0 0 0 c3 0 0 0 c> rl ri d r-i 0 0 0 0 0 00 0 0 00 00 0 0 0 0 0 0000 000 0 d rl rl rl 0 0 0 000 0 00 r i hl CJ 0 00000 0 0 000 0 0 0 00 0 0 0 0 0 hi cv N c\1 hi (v 0 m e l cu 0 01 N m cn co m hl CJ 0 hl h i m 00 00 0 m YO a, 07 m 0 co co 0 m m QD 0 m 0 b cn a, co 3 rl f m a, a, 0, a, co f rl f UJ a, cn a, cn a, cn cn a, cn cn a, cn cn cn cn cn cn cn a, a, . . .c3. . . . . . . . . . . . . . . 0 0 0 0 0 00 0000000000 (u c, 0 b 3 r-l rl h l f N b f 0 Q, a3 0 rl OD cr) 0 0 0 c3 0 0, cn cn a 0 0 co b r- a3 CO cn CJ cv N c4 . (v d rl rl rl CJ hl rl rl i-l rl d rl rl 0 0 0 c> 0 0 0 0 0 0 0 0 0 0 0 0 0 0 * 0 +JVI .................. a c, Rl 0 0 0 c3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 J cn F: 0 rl rl a fm (v c3 (* 0') cn 0, rl f hi f CJ (v Ln 0 CD f CD 0 f CJ Cr) hi CJ 0 4 m m v) .................. Lo d Lo m m m (D mm 0 0 0 c3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 v) rd 3 x El 0 Qi rd c, a c7 J I I j 03 J a) rl A a E-c ... -80- -- , I ‘cl E I ii x -4 0 0 0 c l 0 f f ~ c n ~ ~ L o m L o a a f f f f cocoCD~bcococoaLomLocow~cocococococo b F F ~ . F P F c n m ~ m d r l r l r l ~ F b t - F r l r l r l ~ l r l r l r l r l r l r l r l ~ c v h l c v c v r l r l r l r l ................ ooocloooooooooooooooo . . . ? I ooocboooooooooooooooo 3 0 rl F4 c a, M 0 & +J -d 2 n Lo 0 z k”0 u c 0 +J cn cr) m m co m co cv m G co a ii ~lcvrlrlcoLocvrlfmcvrlrl0000 51 a C.D.f m . . . . . . . . . . . ....... ooooocoooooooooooooo Lo Lo a, f rl t- rl m (u b rn a c a cn c 0 rl rl cv U) c v o rl f 0 0 f m CD b In F) 0 fOcv30LomF0fmcoLomcofa0F)In o r l ~ ~ i c v ~ c v o ~ c v ~ ~ r l c v h l m ~ ~ c o c o 4 a0 0 rn rn .................... a c 0 0 0 C)0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 & 0 ccr a C’ rd 0 a rl *d p c m a $ d L cn Q) rl A a E-c &I -81- J J +J c 0 0 bl 0 4 a m P 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0000000000000000000000000 0000000000000000000000000 d d d r l r l r i ~ r l r l r l r l r l m o m m o m o o m m o o o .J ; 1 P U J u x E 0 m x E 0 U m Q) 00000000000000000000000c0 O O O O O c > o O O O O O O O O o O O O O o o o o o O O O O O C ~ O O O O O O O O O O O 0 O O O O O O O ......................... d N N N N N ~ ~ N N N N N N N N N N N C V N N N N N ~ ~ d I E c, m J a E a a rl rd 9-l m P 4 m ! o fd -4 3 c 4 r o P J d z c 3 p: -82- I li s 0 0 0 0 0 0 0 0 0 0 0 0 0 ooooooocooooo 0 0 0 0 0 0 0 0 0 0 0 0 0 f f j f f f 3 f j f f f f r-r-fimmmmmmmmm baaammmmma3ma3a3 ar-r-r-mcnmmcndr-idr-i b d r - i l - i d d d d d m m m m ............. d 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 a u a, m u u oooooooocoooo 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 ............. m N N m m m N N m m N m N d o m o l - l F o m m ~ m w m m m m m o m m m a d m o a 3 f m N d 3 N m d d f N m r - i ............. 0 0 0 0 0 0 0 0 0 0 0 0 0 m o w r l l n m a 3 a o o o d o mmlnNmfa,mfmNal-4 ............. NddrlC9C'Jddd2tmC'4N ooooooooa3oooo Q) c I .rl n 0 d 0 A z c I 3 d a, d a 3 -83- 0 I x I Cr) a, ooc~oocooooooooooooooooo Fc 0 0 0 G 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 a ooc'oooooooooooooooooooo r l r l ~ l r l r l ~ r i r i r l N r n C J N C J ~ C J f f f ~ f f ~ F: rd a, t: ....................... 00,000000000000000000000 fcnLor.0co0m000000000000000 o m c n m o c n o m o o o o o o o o o o o o o o o ...................e... f o m m f m f m f f ~ ~ f f f f f f f f f f f s c 3 I z -84- 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 d d r l r l 4 d m o m C Q o m f w c n L n W ( r 1 0 03 m 3 c n m c o m c n c V C l m c n o m = l - c o b c o b c D m = t - m c n m O m b m b O o m b P J m o . . . . . . . . . . . . 0 0 0 d 0 0 0 0 0 d 0 0 0 0 0 0 0 0 0 0 0 0 0 0 a r k 0 u+ a IJ a o o o o o o r l o o o o o . . . . . . . . . . . . 0 0 0 0 0 0 0 0 0 0 0 0 f f f f f f f f f f f f a tu rl a, -4 A a I3 -85- X m li X I 3 0 rl r.4 0, Fc a, v a 5 c\I v) Loo II II II w o m o w c m c a o m o c \ I w m b N a m L o @ J u l w .. o m 0 o a m CD 0 . . . . . . . . . . . . d r f l ~ r 0 0 l 0 0 f 4 c J 0 r 0 l 0 O I f C - i u 0 l 0 - l 0 II n *I 3rl pcul =k a c: a 0 0 L 0 0 o L 0 0 o 0 0 v 0 0 ) L 0 0 o 0 0 o o 0 0 o 0 0 o 0 0 ~ m 0 0 L 0 0 o m r l l - l r l r l l - l l - i r l r l cn a u *#-I rl *ti m a a 3 crd a, r: d 4 a b m m v ) c D m 3 m m r r ) m l - i a m L o f m ( v f f b ? l 3 c, c, 3 L o m d a m N a m c D a m . . . . . . . . . . . . 0 0 0 N 0 0 0 0 0 0 0 0 0 a 0 0 0 0 0 0 0 0 0 0 0 0 0 c, a a .ti 0 0 r - L o m ~ O ( v m r l f f m O O L o ( v d m m m m h l rl 0 . . . . . . . . . . . . pc [I) F: 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 a J 0 0 r= 3 Fc 3 0 % rd v a n 3 0 J rl EL( m rl .I a, z O1 rl J A a I I 3 -86- d tc Fc Q) c, id 3 0 z z O O O O O O O O O O Q O O O O O O O O O O O O O O 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 o o a o o ~ L o m L o ~ m ~ a ~ ~ ~ ~ ~ 0 0 0 Lo rlrlrll-irlcvcvmwwmcv 0 u a 0 0 0 E: a m a u *ti d -rl m , a cv co o m 0 a3 a,0307 LnfOrna,frtO 00 m O c v ~ N ~ b O O L o Q m c v c - ~ c - f ~ m c o b m a , ~ mco03mWmcvfm0ammcvmOcvNmfm~cvl~Cu 0 0 0 0 0 b 0 0 0 0 0 f 0 0 a 0 - 00 0 0 0 0 0110 0 c, c, C ......................... a 0000000000000000000000000 Q) c, a a 0.4 rl 0 0 W a , m ~ 0 3 m a , o o o ~ ~ c v ~ ~ ~ c v o o b c o c o ~ . m ~ ~ ( D c o r n f ~ ~ ~ ~ ~ O m c o o m E: 0 u a ......................... 000000000000000000d000000 0000000000000000000000000 E: 5 k 0 Ict a a +J a 3 0 f ri Q) d c1 a E-c -87- 3 0 rl r.4 & a, c, a 3 EmE 0 0 a c a G a, M 0000000000000 0000000000000 0000000000000 mmmmtwmmmmmmmm E c, .rl z h CD rl 0 z a, h 0 u a Qq 2 rn cn rd 0 0 *rl d *rl I cn a 5 c, c, 3 4 g 0 0 a a, c, a a *ti d 0 v) F: 0 0 c 3 m d a o m C D m m 3 ~ m m b d m m m m m m m 3 m N m 3 0 ............. 0 0 0 0 0 0 0 0 0 0 0 0 0 O O O O O O O O O O O O O s4 0 (H . a c1 a N .. bU0"I * Ea0Y s: 0 +I L4 m rl 0 z Q) d A f F : d a €+ -88- 7 CG I 30 ri b-l ri 0 c a +Ju 0 I W co co W W W ~ O f r i f 0 ~ m 0 f r i f 0 0 0 0 f r i ~ 0 O hl ..................... mrnocooot-~oocooocow~oLDo~rl n cr i 0 N r i 0 ~ ~ 0 0 N r i 0 r i N ~ ~ c l r i O d N ~ Lo Lo rlrl 2 0 z a 0 0 a c a cn a 0 *rl ri -rl -1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2 Fc c a al 000000000000000000000 m L O m m m m m 0 0 0 0 0 0 0 0 0 0 0 0 0 0 rlridrlridrlcl@lCJNhlNN c *d a k c5 u u a \ bc cn a 3 m c, u CJ 0 a a, ~ ~ r n N o ~ m ~ O ~ N m r i L O t - f ~ t - ~ O c o r i ~ f W O C D ~ t - ~ t - ~ ~ t - O f L O L o ~ ~ r n O rndf~fdd~rirnt-O~CJNOc-mNNCJ ..................... 3,12 000000000000000000000 M 000000000000000000000 a P a a -rl rl t - 0 0 0 m 0 0 0 m ~ Q 0 0 0 (I) c 0 0 c 04 Q ~ 0 0 N ~ ~ m 0 0 ~ ~ 0 0 0 ~ 0 0 0 0 f N N c ..................... ~ r l ~ ~ 0 0 f ~ d 000000000000000000000 3 SI 0 +I a c, fd n 8 T I F4 LD ri QJ d A a w -89- l 0 0 ~ c ~ - h ~ l ~ J .d i 9.2 Core Data J J .J J J 3 J -904 N l l c-4 N ri rl N c4 0 rl CJ N N hl o m m . . . . . o C I ( D m D I L D N O O O a, a N N C3 W cv 3 m m N c 0 *rl f +, .rf hl CJ [I) 0 0 0 m N N N I ri I N rl I c-4 cn -91- J 9.2- 1- 3 D e s c r i p t i o n : The M a s s i l l o n s a n d s t o n e i s found i n Holmes County, Ohio, and h a s been e x t e n s i v e l y q u a r r i e d for a v a r i e t y of p u r p o s e s . The s t o n e is medium- to- coarse .J g r a i n e d and i s composed m s t l y of q u a r t z g r a i n s , which are s u b a n g u l a r t o subrounded i n s h a p e . The cementing materials d' a r e i r o n o x i d e , c l a y m i n e r a l s , and s e c o n d a r y s i l i c a . T e s t s made for t h e Briar Hill S t o n e Company show t h a t t h e s t o n e h a s a n a b s o r p t i o n of water of a p p r o x i m a t e l y 6 % b y weight. .J The c r u s h i n g s t r e n g t h r a n g e s from 4 0 0 0 t o 6 0 0 0 p s i , 5000 p s i being about average. p e r cubic foot. The s t o n e weighs 1 3 5 pounds The a v e r a g e p e r m e a b i l i t y of t h e s a m p l e s J used i n t h i s s t u d y w a s 8 0 0 md, and t h e a v e r a g e p o r o s i t y a b o u t 22%. 9.2- 2 Uncons'olidated O t t a w a S i l i c a 9.2- 2- 1 Physical Properties Core No. 14 15 16 17 Length, c m 5.696 5.590 5.657 5.894 C r o s s - S e c t i o n a l Area, c m 5.067 5.067 5.067 5.067 Average G r a i n S i z e , mm (35- 45 mesh) (80- 100 mesh 1 1 (80- 100 (80- 100 mesh) mesh) J 3 9.2.2- 2 M i n e r a l o g i c a l Composition Weight % 99.806 Silicon dioxide (SiO,) Aluminum o x i d e (A1203) 0.047 I r o n oxide (Fe203) 0.019 Titanium dioxide (Ti02) 0.018 Calcium o x i d e ( C a O ) <o. 01 Magnesium o x i d e (MgO) <0,01 3 4 0.09 Loss on I g n i t i o n (LO11 - 92- J 9.2- 2- 3 D e s c r i p t i o n : The O t t a w a s a n d used i n t h i s s t u d y i s t h e No. 1 7 s i l i c a g r a d e and i s c o m m e r c i a l l y a v a i l a b l e from t h e O t t a w a D i v i s i o n , P a r k e r I n d u s t r i a l and Foundry S u p p l y , Rurlingame, C a l i f o r n i a . I t i s more t h a n 9 9 % w e i g h t q u a r t z and t h e g r a i n s a r e f a i r l y w e l l rounded. The d i s t r i b u t i o n of g r a i n s i z e s i s as f o l l o w s : U.S. Opening, ! l i l l i m e t e r P e r c e n t Weight R e t a i n e d 40 0.420 8.1 50 0.297 44.5 70 0.210 28.8 100 0.149 12.7 140 0.105 4.4 200 0.074 1.1 270 0.053 0.2 Sieve No. The s a n d w a s s i e v e d and o n l y u n i f o r m l y s i z e d g r a i n s w e m used t o p r e p a r e a core f o r t h i s s t u d y . -93- 9.3 D e r i v a t i o n of E q u a t i o n s -94- 9.3- 1 C a p i l l a r y Tube V i s c o m e t e r : Because l i q u i d v i s - c o s i t y d a t a o b t a i n e d f r o m s u p p l i e r s are a v e r a g e p r o d u c t q u a n t i - t i e s and t h o s e from c o n v e n t i o n a l r e f e r e n c e s were n o t g i v e n at h i g h working t e m p e r a t u r e s , it was n e c e s s a r y t o d e t e r m i n e v i s c o s i t y v e r s u s t e m p e r a t u r e a t o p e r a t i n g pressures. A c a p i l l a r y t u b e v i s c o m e t e r , whose o v e r a l l l e n g t h w a s 62.875 i n c h e s and whose i n t e r n a l d i a m e t e r was 0.033 i n c h e s , w a s c o n s t r u c t e d from a 316 s t a i n l e s s s t e e l t u b e . c o e f f i c i e n t of t h e r m a l e x p a n s i o n w a s 8 . 9 x The l i n e a r in/in-OF. The l a m i n a r f l o w o f l i q u i d s t h r o u g h c i r c u l a r c o n d u i t s obeys P o i s e u i l l e ' s l a w : ' 4 rr Ap = 8pR where q = f l o w r a t e , cc/sec; r = i n s i d e r a d i u s , cm; Ap = p r e s s u r e d r o p , d y n e s / c m2 ; ?J = liquid viscosity, poises, 2 = l e n g t h of c a p i l l a r y , c m . For r and R i n i n c h e s , Ap i n p s i , and i n cp u n i t s , Eq. 9 - 1 becones: q = 4.437 x 1 0 7 r 4 A2 (9-2) RP and ?J (9-3) = 0 . 5 2 3 0 !& 9 Knowing t h e a c t u a l v a l u e o f v i s c o s i t y a t 7OoF, and f r o m measurements of t o be 0.5113. p and q , t h e m u l t i p l y i n g c o n s t a n t w a s f o u n d Therefore: '70 = 0.05113 -95- % (9-4) p, T h e r e f o r e , a graph of Y = Ap (l+--) b Dm ;&a Pa vs 9, .x J a 1 (1+b prn s h o u l d y i e l d a s t r a i g h t l i n e o f s l o p e rj and i n t e r c e p t E 1 , d p r o v i d e d t h a t t h e v a l u e of b is known. J J 3 J J J J J E q . 9- 10 was t h e w o r k i n g e q u a t i o n for t h i s a p p a r a t u s . The r e s u l t s a g r e e c l o s e l y w i t h t h o s e found i n t h e I n t e r n a t i o n a l Critical Tables. 39 9.3-2 V i s c o - I n e r t i a l Flow o f G a s : The q u a d r a t i c e q u a t b h as proposed by F o r c h h e i m e r and m o d i f i e d by C o r n e l l and Katz (see r e f s . 1 0 and 11) i s : -8= avq + BPq 2 (9-11) for t h e case of v i s c o - i n e r t i a l flow o f g a s . For v i s c o u s flea, t h e q u a d r a t i c t e r m o f 9 - 1 1 i s small enough t o b e n e g l e c t e d , and a h a s t o b e t h e r e c i p r o c a l o f p e r m e a b i l i t y , i . e . , Q = l/k. The i n t e g r a t e d form o f E q . 9 - 1 1 f o r h o r i z o n t a l l i n e a r flow i n t h e a b s e n c e of s l i p p a g e i s : When t h e r e i s g a s s l i p p a g e , a becomes ):+ kl( _I b k(l+- and s i m p l i f y i n g , Pm or Y = E + fix -97- 1 b ' R e p l a c i n g a by A t t e m p e r a t u r e s , T , o t h e r t h a n room t e m p e r a t u r e , t h e l e n g t h of t h e t u b e i s : (9-5) and rT 4 = r 7 0 ‘[l + B (~-7011~ (9-6) or (9-7) Because B , t h e l i n e a r c o e f f i c i e n t of t h e r m a l e x p a n s i o n , i s small, Eq. 9- 7 c a n be approximated as: 4 4 ’-T= - ‘T r70 ‘70 6 + 3B ( T - 7 0 1 7 For t h e a p p a r a t u s : UT = 0,05113 l l + 2 . 6 7 x (T-70)3 Q (9-9) T h e r e f o r e , t h e v i s c o s i t y a t any t e m p e r a t u r e i s : (9-10) Where : aT = 0 . 0 5 1 1 3 l l t 2 . 6 7 x 10’’ -96- (T-7011 9.4 L i s t of M a n u f a c t u r e r s -99- LIST OF YANUFACTURERS The f o l l o w i n g i s a l i s t of t h e v a r i o u s p i e c e s of e q u i p ment or s u p p l i e s t h a t were used i n t h i s work, t o g e t h e r w i t h t h e c o r r e s p o n d i n g names of m a n u f a c t u r e r s a n d / o r s u p p l i e r s from whom t h e y were a c q u i r e d . Chevron White M i n e r a l O i l N o . San Francisco. 3 - Van Waters E Rogers, I n c . - Pressure Transducers D y n a s c i e n c e s Corp. , Model KP 1 5 , c/o Gaco I n s t r u m e n t S a l e s , 655 Castro S t r e e t , S u i t e 2 , Mountain V i e w , C a . , 94040 ( 9 6 1 - 2 2 2 2 ) . B a r n e t t I n d u s t r i a l Dead Weight T e s t e r - c / o Gaco I n s t r u m e n t , 94040 Sales, 6 5 5 C a s t r o S t r e e t , S u i t e 2 , Mountain V i e w , C a . (961-2222). P r e s s u r e I n d i c a t o r - Pace Node1 CD 25, c / o Gaco I n s t r u m e n t S a l e s , 6 5 5 C a s t r o S t r e e t , S u i t e 2 , Mountain V i e w , C a . , 9 4 0 4 0 (961-2222). P r e s s u r e R e g u l a t o r - V o l u m e t r i c s , Model V R C - 4 0 0 , 1 0 2 5 A r b o r Vitae S t r e e t , Inglewood, C a . , 90301 ( 2 1 3 ) 6 4 1 - 3 7 4 7 , o r c / o Gaco I n s t r u m e n t S a l e s , 6 5 5 C a s t r o S t r e e t , S u i t e 2 , F o u n t a i n V i e w , C a . , 94040 ( 9 6 1 - 2 2 2 2 ) . - High P r e s s u r e R e g u l a t o r Newark, C a . (793-2559). Model 4-580, Matheson Gas P r o d u c t s , - V a r i a b l e R a t e O i l Pump Model PC, Whitey Tool E D i e Company, 3 6 7 9 Landregan Emvl., Oakland, C a , (653-51001, loan from USBM. - H y d r a u l i c Hand Pump E n e r p a c , Model P- 39, P a u l Monroc H y d r a u l i c s , I n c . , 1 5 7 0 G i l b r e t h Road, Burlinganre, C a . , 9 4 0 1 0 (697-2950). - C o n s t a n t R a t e Pump Hand-made e q u i v a l e n t t o Ruska 2 2 0 0 s e r i e s . Uses Viton 0 r i n g w i t h machined t e f l o n b a c k - u p . r i n g . Accumulators ( G r e e r o l a t o r ) , Model No. 20- 30 TMR-S-% WS, Hyd r a u l i c C o n t r o l s , I n c . , 1330 6th S t . , E m e r v v i l l e , C a . , 94608 (658- 8300). Recording P o t e n t i o m e t e r (for t e m p e r a t u r e ) Model Speedo Max v, Leeds E N o r t h r u p , 1 0 9 5 Market S t . , S a n F r a n c i s c o , C a , (349-6656). 3- -100- - Thermocouples I r o n - C o n s t a n t a n , C o n a x , c / o I n s t r u m e n t Labo r a t o r y , 6 4 4 Emerson S t . , P a l o A l t o , C a . , 9 4 3 0 3 ( 3 2 8 - 1 0 4 0 ) . - Temperature C o n t r o l l e r API Model 2 2 8 w i t h 4 0 1 0 Power P a c k , A P I I n s t r u m e n t s , 2339 C h a r l e s t o n R d . , Mountain V i e w , Ca., 94040 (964-0512). - L a b o r a t o r y Flowrator K i t Model No. 10A3565ALK2, F i s h e r E P o r t e r C o . , 1 3 4 1 North Main S t . , Walnut Creek, C a . , 94596 (933-8880). Core S l e e v e - V i t o n A t u b i n g , \?‘estAmerican Rubber Co., North Main S t . , O r a n g e , Ca., 9 2 6 6 8 ( 7 1 4 - 5 3 2 - 3 3 5 5 ) - 750 - 0 !ings V i t o n A w i t h t e f l o n b a c k - u p r i n g s , ABSCOA I n d u s t r i e s , 8 8 0 B u r l i n g a m e A v e . , Redwood C i t y , C a . (369-4897) OR 1 0 7 1 W. Arbor Vitae S t . , Znglewood, C a . , (213- 7764561). - Tubin T u b e s a l e s , 5 0 0 Sansome S t . d l 9 1 9 ) . , S a n F r a n c i s c o , Ca. F i t t i n g s E V a l v e s - Van Dyke E F i t t i n g C o . , Oakland, C a . (658-1700). 5 5 2 5 M a r s h a l St., Gas A n a l y z e r - Gas Master, Laboratory Model, GOW-MAC I n s t r t k ment C o . , 1 0 0 Kings F.d., M a d i s o n , N . J . 0 7 9 4 0 (201-377-34501 o r A p p l i e d I n s t r u m e n t C o . , 1 9 9 1 s t S t r e e t , Los A l t o s (941-592k3). - Recording P o t e n t i o m e t e r ( f o r p r e s s u r e ) r e c o r d e r , L e e d s and N o r t h r u p , BD-9, P.O. Ca. (593-8392). Two pen m u l t i - r a n g e Box 6 3 4 , B e l m n t , - Alundum Core N o r t o n Co., I C D , 2555 L a y a f e t t e S t . , Clara, C a . 95050 ( 2 3 4 - 7 7 1 0 ) . Santa - Lapp P u l s a f e e d e r Pump Model LS- 20, 316SS, 1 / 6 h p , 94 Natoma S t . , S a n F r a n c i s c o , Ca. 94105 ( 3 9 1 - 7 6 5 0 ) . O t t a w a S i l i c a , No. 1 7 S i l i c a , P a r k e r I n d u s t r i a l and F o u n d r y S u p p l y , 1 8 8 1 R o l l i n g Rd., Burlingame, C a . , 94010 ( 6 9 7 - 8 8 6 5 ) . Massillon S a n d s t o n e - T h e B r i a r H i l l S t o n e C o . , Ohio, 4 4 6 2 8 ( 2 1 6 - 2 7 6 4 0 1 1 ) . -101- Glenrnont, NOMENCLATURE 10. English A = area, c m 2 k = p e r m e a b i l i t y , md L = l e n g t h of c o r e , c m p = pressure, p s i q = flow r a t e , cc/sec w = flow r a t e , g m / s e c T = temperature, 0K or OF r = radius, c m v = flow v e l o c i t y , cm/sec Greek p = d e n s i t y , gm/cc u = viscosity, cp 4 = porosity, fraction A = increment Subscr i D t s a = atmospheric condition c = c o r e or c o n f i n i n g m = mean v a l u e T = temperature -102-