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The production of uniform sized drops in liquid-liquid systems Izard, John Arthur Whitaker 1962

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THE PRODUCTION OF UNIFORM SIZED DROPS IN LIQUID-LIQUID SYSTEMS by JOHN ARTHUR WHITAKER IZARD B. Eng. (Chem.) M c G i l l U n i v e r s i t y 1946 A THESIS SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF APPLIED SCIENCE i n the Department of CHEMICAL ENGINEERING We accept t h i s t h e s i s as conforming t o the r e q u i r e d standard. The U n i v e r s i t y of B r i t i s h Columbia October, 1962 In presenting this thesis in. partial fulfilment of the requirements for an advanced degree at the University of British Columbia, I agree that the Library shall make i t freely available for reference and study. I further agree that permission for extensive copying of this thesis for scholarly purposes may be granted by the Head of my Department or by his representatives. It is understood that copying or publication of this thesis for financial gain shall not be allowed without my written permission. J . A. I z a r d . Department of Chemical Engineering The University of British Columbia, -Vancouver 3, Canada. NOV 10 1962 Date i i ABSTRACT The p r o d u c t i o n of u n i f o r m - s i z e d drops without s m a l l f o l l o w e r drops or " t r a i l e r s " i n l i q u i d - l i q u i d systems was s t u d i e d u s i n g a p e r i o d i c i n j e c t i o n technique f o r d i s p e r s i n g one l i q u i d through a sharp edged nozzle i n t o the other. Previous i n v e s t i g a t o r s u s i n g a continuous f l o w technique found that uniform s i z e d drops without t r a i l e r s were l i m i t e d t o systems of higher i n t e r f a c i a l t e n s i o n . The e f f e c t s of nozzle i n s i d e diameter,, nozzle m a t e r i a l , and of v e l o c i t y - t i m e p r o f i l e of the dispersed f l u i d through a nozzle at drop formation v/ere examined using> , two systems; n-butanol and water of very low i n t e r f a c i a l t e n s i o n , and methyl i s o b u t y l ketone and water of low i n t e r -f a c i a l t e n s i o n . These two systems were chosen so t h a t the r e s u l t s of t h i s study could be i n t e g r a t e d w i t h other work. The v e l o c i t y - t i m e p r o f i l e s were obtained by u s i n g a p o s i t i v e displacement bellows pump, the stroke of which was c o n t r o l l e d by a cam f o l l o w e r through a v a r i a b l e r a t i o l i n k a g e u s i n g three d i f f e r e n t cam p r o f i l e s . The c o n d i t i o n s under which uniform s i z e d drops ;" without t r a i l e r s were formed, were l o c a t e d f o r both systems. r The e f f e c t s of surface a c t i v e contaminants and the w e t t i n g of the nozzle t i p by the d i s p e r s e d phase were considered. x i i ACKNOWLEDGEMENTS The author wishes t o acknowledge the as s i s t a n c e he has r e c e i v e d I n t h i s research from Dr. J . S. F o r s y t h and Dr. S. D. Cavers•. He a l s o wishes t o acknowledge" the f i n a n c i a l a s s i s t a n c e given by the N a t i o n a l Research C o u n c i l of Canada. i i i TABLE OF CONTENTS Page INTRODUCTION 1 EXPERIMENTAL INVESTIGATION 11 I PRELIMINARY INVESTIGATION 11 (A) SCOPE 11 (B) APPARATUS 11 (C) PROCEDURE 17 I I MAIN INVESTIGATION 21 (A) SCOPE 21 (B) MODIFICATIONS TO ... . EXISTING APPARATUS 22 (I) D e s i g n o f pump and . c a l i b r a t i o n 22 ( i i ) Pump mechanism 27 ( I i i ) Cams 28 ( i v ) P i p i n g m o d i f i c a t i o n s 37 ( v j O p t i c a l m o d i f i c a t i o n s 37 (6) EXPERIMENTAL WORK WITH THE _ . N-BUTANOL AND WATER SYSTEM 48 ( i ) C h a r g i n g t h e . ; a p p a r a t u s 48 ( I I ) E x a m i n a t i o n o f drops p r o d u c e d w i t h s t a i n l e s s s t e e l n o z z l e s 49 ( i i i ) E x a m i n a t i o n o f drops p r o d u c e d w i t h b r a s s n o z z l e s 55 ( i v ) E x a m i n a t i o n o f drops produced w i t h T e f l o n -t i p p e d n o z z l e s J6 i v Page (D) EXPERIMENTAL WORK WITH . METHYL ISOBUTYL KETONE AND WATER-SYSTEM. . . 8 l RESULTS AND DISCUSSION 96 CONCLUSION 112 SUGGESTIONS FOR FURTHER STUDY 114 APPENDICES Appendix A 116 Appendix B 117 REFERENCES 118 V LIST GP FIGURES FIGURE PAGE 1. Oblate spheroid drop shape ...... 4 2. Apparatus f o r the P r e l i m i n a r y I n v e s t i g a t i o n 12 3. Diagrammatic layout of apparatus, P r e l i m i n a r y I n v e s t i g a t i o n 13 4. O p t i c a l arrangement, P r e l i m i n a r y I n v e s t i g a t i o n 18 5. Hoke 1/8 i n . bellows s e a l needle valve 23 6. Bellows valve pump 24 7. Pump d r i v e components 29 8. Cam operated a d j u s t a b l e stroke mechanism 30 9. Cam f o l l o w e r 32 10. Cam "A" 33 11. Cam "A" and "B" 34 12. Apparatus 39 13. Mounted F r e s n e l lens 41 14. Revised m i r r o r arrangement 43 15. P o r t a b l e m i r r o r holders 44 16. Apparatus set up w i t h Bo l e x H16 R e f l e x Camera 46 17. Runs 14 t o 24. Types of drops produced, l / 8 i n . I.D. s t a i n l e s s s t e e l n o z z l e , Cam "A" forward, n-butanol and water 52 v i FIGURE PAGE 18. Run 35 • Types of drops produced and r e g i o n of s i n g l e drops, 5/32 i n . I.D. s t a i n -l e s s s t e e l n o z z l e , Cam "A" reversed, n-butanol and.water... 54 19. Run 38. Types of drops produced and r e g i o n of s i n g l e drops, 5/32 i n . * I.D. brass,, n o z z l e , Cam "A" forward, nr-butanol and water 57 20. Run 39. Types of drops produced and r e g i o n of s i n g l e drops, 5/32 i n . I.D.. brass. , , ., n o z z l e , Cam "A" reversed, n-butanol and water.. 58 21. Run 40. Types of drops i produced and r e g i o n . o f . s i n g l e drops, 5/32 i n . I.D. brass n o z z l e , Cam "A" forward,, 1/4,in. spacer, n-butanol and water 59 22. Run 41. Types of. drops. .„,., produced and r e g i o n of s i n g l e -drops, 5/32 i n . I.D., brass, , n o z z l e , Cam "B", n-butanol and water...................,., 60 23. Run 42.. Types of, drops. produced and r e g i o n of s i n g l e drops, 5/32, In.., I.D... brass n o z z l e , Cam "A" forward ( r e p a i r e d ) , n-butanol and water. 61 24.. Run 43. " Types of. drops .. . t. r t t produced, 1/8 i n . I.D. brass nozzle,, Cam "A" forward,, , s . . , n-butanol and water 62 25. Run 44. Types of drops . ,„ f. ; produced, 1/8 i n . I.D. brass n o z z l e , Cam "A" reversed, n-butanol and water,. 63 v i i FIGURE PAGE 26. Run 4 5 . Types of drops . produced,, 3/16 i n . , I.D. brass • ' n o z z l e , Gam "B", n-butanol and water. 64 27. Run 46. Types of drops produced, 3 / l 6 i n . I.D. brass n o z z l e , Cam "A" forward, n-butanol and water 65 28. Run 4 7 . Types of 'drops produced, 3 / l 6 i n . I*D. brass n o z z l e , Cam "A" reversed, n-butanol and water. 66 29. Run 5 ! . Region of s i n g l e drops, 11/64 i n . I.D..brass, n o z z l e , Cam "A" forward, n-butanol and water. 67 30. Run. 52 . Regions of, s i n g l e drops,.11/64 i n . I.D.,brass n o z z l e . Cam "A" reversed, . . ., n-butahol and water 68 3 1 . Run 53 . Region of s i n g l e drops, 11/64 i n . I.D. brass n o z z l e , Cam "B", n-butanol and water...,..,..;..........,.. 69 32. Run 54 , r e p e t i t i o n of Run 5 1 . Region.of s i n g l e drops, 11/64 i n . I.D. brass„nozzle, Cam "A" forward, n-butanol and water.... 70 33 . Run 55, r e p e t i t i o n of Run 53 . f> Regions of s i n g l e drops, 11/64 i n . I.D. brass, n o z z l e , Cam "B" n-butanol and water..,.....' 71 34 . E f f e c t s of Contamination Run 53 , Frame 20 , before con-t a m i n a t i o n , Run ^ ^ F r a m e 2 1 , a f t e r contamination. 73 v i i i FIGURE PAGE 35. Run 48. Types of drops produced, 11/64 i n . I.D. ''Teflon" nozzle,' Gam "A" forward, n-butanol *and w a t e r . . • .78, 36; Run 49. Types of drops produced,. 11/64 i n . I.D. "Te f l o n " n o z z l e , Cam "A'J reversed, n-butanol and water... 79 37. 11/64 I n . I.D. "T e f l o n " t i p p e d n o z z l e , n-butanol and water..... 80 38. Bellows pump......... ** * * . . 84 39; Run 57; Region of s i n g l e drops, 1/8 i n . I.D. brass n o z z l e , Cam "A" reversed, methyl i s o b u t y l ketone and water;*.**... 86 40; Run 58* Region of s i n g l e drops, 1/8 i n . I.D. brass n o z z l e ; Cam "A" forward, .methyl i s o b u t y l ketone and water.*.*..* 87 41* Run 59. Region of s i n g l e drops, 1/8 i n . I.D; brass n o z z l e , Cam "B", methyl i s o b u t y l ketone and*water. ;**.*. * 88 42. Run 60; Region of s i n g l e ' drops, 11/64 i n . I.D. brass 1 n o z z l e , Cam "B", contaminated methyl i s o b u t y l ketone and water.. 89 43. Run 63. Region of s i n g l e drops-, 11/64 i n . I.D.. brass n o z z l e , Cam "B", methyl* ..•>•, I s o b u t y l ketone and water......... 90 44. Run 64. Region of s i n g l e drops, 11/64 i n . I.D. brass n o z z l e , Cam "A" forward,-methyl. I s o b u t y l ketone and water. 91 i x FIGURE PAGE 45. Run 67. Region of single drops, 7/64 i n . I.D. brass nozzle, Cam "A" forward, methyl i s o b u t y l ketone and water....... 92 46. Run 68. Region of single drops, 5/32 i n . I.D. brass nozzle, Cam "A" forward, methyl i s o b u t y l x ketone and water 93 4 7 . Run 36 , Frame 3 , Single Drops without T r a i l e r s ••••>• 99 48a. Run 37* Frame 15, Single Drops, without T r a i l e r s 100 48b. Run 37* Frame 16, Single Drops without" T r a i l e r s 100 4 9 a . Run 4 2 , Frame 2, Single Drops without T r a i l e r s 101 49b. Run 4 3 , Frame 15, Single Drop and.One T r a i l e r . . . 101 50a. Run 46, Frame 9* One Drop and Two T r a i l e r s 102 50b. Run 51 , Frame 22, Single Drop without T r a i l e r s 102 51a. Run 56, Frame 4, Single Drop without T r a i l e r s 103 51b. Run 56, Frame 13, Single Drop xvithout T r a i l e r s 103 52a. Run 67 , Frame 4, Single Drop without T r a i l e r s * 104 52b. Run 68, Frame 6, Single Drop without.Trailers 104 X FIGURE PAGE 53 E f f e c t of Cam Spacer, Figures 21 and 22 superimposed, n-butanol and water.. 107 54 S t a i n l e s s s t e e l and brass n o z z l e s , F i g u r e s 18"and'20 super-. imposed, n-butanol. and water.... 108 x i LIST OF TABLES Key t o Figu r e 1.. ... Key t o Figure 3....... Key t o Figure 4... C a l i b r a t i o n of 1/8 i n . Hoke Bellows S e a l Valve #432 Key t o Figure 8 Key t o Figure 12. Runs made w i t h brass nozzles w i t h n-butanol-water system Surface Tension Measurements.... D. Experimental I n v e s t i g a t i o n Methyl I s o b u t y l Ketone-Water System Measurement of drop s i z e s by p r o j e c t i o n on graph paper u s i n g a s l i d e - s t r i p f i l m p r o j e c t o r . INTRODUCTION Although throughout t h i s century a considerable amount of a t t e n t i o n has been given t o the study of drops and bubbles i n g a s - l i q u i d systems, only i n the l a s t three decades has much i n t e r e s t been shown i n s t u d i e s of drops i n l i q u i d - l i q u i d systems. As the present i n v e s t i g a t i o n i s concerned w i t h t h i s l a t t e r f i e l d , only p e r t i n e n t l i t e r a t u r e on drop formation i n l i q u i d - l i q u i d systems w i l l be considered. Hayworth and T r e y b a l ( l ) s t u d i e d the formation of drops f o r the continuous f l o w of one l i q u i d i n t o another through sharp-edged n o z z l e s . Prom t h i s study, they developed a s e m i e m p i r i c a l equation f o r c a l c u l a t i n g drop s i z e based upon a f o r c e balance -during drop formation on the t i p of a n o z z l e . For noz z l e flow v e l o c i t i e s up t o 10 cm. per second t h i s equation p r e d i c t e d the diameter of the drops produced, and from 10 t o 30 cm. per second, the diameter of the l a r g e s t drops produced. Drop s i z e was found t o be "uniform" and t o incr e a s e I n s i z e w i t h i n c r e a s e i n v e l o c i t y up t o 10 cm. per second, and then t o decrease both i n u n i f o r m i t y and i n s i z e w i t h f u r t h e r increase i n v e l o c i t y from 10 t o 30 cm. per second. Above 30 cm. per second drop s i z e was very "non-uniform". They a l s o observed t h a t at c e r t a i n v e l o c i t i e s a very s m a l l drop below each l a r g e r drop was formed. 2 K&ftttn and Hixson (2 ) p l o t t e d drop s i z e d i s t r i b u t i o n of toluene dispersed i n water and showed t h a t f o r a 4 .33 mm. I.D. g l a s s nozzle and a toluene flow of 1.50 cc. per second (a n o z z l e v e l o c i t y of 10 .3 cm. per second) there was more than 10$ d e v i a t i o n from the mean f o r 10$ of the drops formed. Apparently, except where flow r a t e s were very s m a l l (up t o 10 cm. per second) and i n t e r f a c i a l t e n s i o n s r e l a t i v e l y l a r g e , the word "uniform" must have been used l o o s e l y when a p p l i e d t o sifcSootfi drops i n both of these i n v e s t i g a t i o n s . K e i t h and Hixson a l s o observed t h a t f o r a given nozzle s i z e and system there was a p a r t i c u l a r flow v e l o c i t y w i t h i n the range of 0 t o 40 cm. per second f o r minimum drop s i z e and maximum i n t e r f a c i a l area. They found t h a t the drop e c c e n t r i c i t y of the oblate s p h e r o i d a l drops, z/x f i g u r e 1, was d i r e c t l y p r o p o r t i o n a l t o the drop s i z e diameter based on a sphere of equivalent volume. They noted t h a t s o l v e n t s of higher v i s c o s i t y and lower i n t e r f a c i a l t e n s i o n would not form i n d i v i d u a l drops from t h e i r l a r g e r n o z z l e s . Lewis, Jones and P r a t t (3) observed t h a t the two h o r i z o n t a l a x i s diameters x and y f i g u r e 1, were equal, and th a t although drops above 1 mm. r a d i u s appeared as o b l a t e spheroids, drops of l e s s than 1 mm. r a d i u s appeared as spheres. Pujinawa, Maruyama and Nakaike ( 4 ) , studying the d i s p e r s i o n of benzene i n t o water, d i s t i n g u i s h e d f o u r patterns of drop formation and r e l a t e d them t o the change i n v e l o c i t y of the emergent benzene. -These patterns were: f i r s t , where the speed was low (below 30 cm. per second) and the benzene column j u s t came i n t o view and drops were formed at the nozzle; second, ("laminar f l o w " from 30 t o 50 cm. per second) where the benzene column incre a s e d up t o maximum height and drops were formed at the top; t h i r d , ("turbulent f l o w " from 60 t o 80 cm. per second) where j e t l e n g t h decreased; and f o u r t h , where the j e t was deformed and very f i n e d r o p l e t s were produced. These phenomena had been reported by ot h e r s , ( l , 2, 5) Siemes and Kauffmann (5) s t u d i e d drop s i z e d i s t r i -b u t i o n a f t e r j e t break-up as a f f e c t e d by i n t e r f a c i a l t e n s i o n and d e n s i t y d i f f e r e n c e between the phases, and by the v i s c o s i t y of the continuous phase. They found a maximum I n t e r f a c i a l area i n the lower v e l o c i t y range as d i d K e i t h and Hixson ( 2 ) . Siemes and Kauffmann (5) a l s o observed t h a t the d i s t r i b u t i o n obtained by d i s p e r s i n g a l i g h t l i q u i d i n t o a heavy one through a nozzle p o i n t i n g upwards was the same as t h a t obtained by d i s p e r s i n g the heavy l i q u i d i n t o the l i g h t e r one through the nozzle p o i n t i n g downwards. Tanweer (6) c o r r e l a t e d drop s i z e w i t h diameter of the o r i f i c e . He r e f e r r e d t o the work of J o s h i (7) who reported t h a t : FIGURE I "OBLATE SPHEROID DROP" SHAPE ( TWO CONJOINED OBLATE SEMI SPHEROIDS ) TABLE 1 Key to Figure 1 Horizontal diameter of drop Horizontal diameter of drop perpendicular to x Semi minor diameter of lower oblate semi spheroid Semi minor diameter of upper oblate semi spheroid h , + hg, minor diameters of the conjoint oblate semi spheroids 6 1. Drop s i z e was Independent of dis p e r s e d f l o w r a t e at very low r a t e s of formation. 2. Volume of each drop increased w i t h decrease i n r e l a t i v e d e n s i t y . 3. Volume of each drop increased w i t h Increase i n i n t e r f a c i a l t e n s i o n . 4 . V i s c o s i t y e f f e c t s were n e g l i g i b l e , only 7$ increase i n volume of drop r e s u l t i n g from a change from 128 t o 1500 c e n t i s t o k e s . N u l l and Johnson (8) obtained a c o r r e l a t i o n which they claimed gave the volume of drops formed from s i n g l e n o z z l e s t o w i t h i n an accuracy of 20$ throughout the range of "uniform" drops. Klee and Tr e y b a l (9) found, as d i d K e i t h and Hixson (2) ana noted e a r l i e r , t h a t f o r a gi v e n system the drop e c c e n t r i c i t y was d i r e c t l y p r o p o r t i o n a l t o the equivalent drop diameter, t h a t I s , t o the diameter of a sphere of the same volume as the drop. They a l s o r e l a t e d t e r m i n a l drop v e l o c i t i e s t o equivalent drop diameters and p h y s i c a l p r o p e r t i e s . Hu and K l n t n e r (10) observed t h a t by p l o t t i n g t e r m i n a l v e l o c i t y against e q u i v a l e n t drop diameter the curve e x h i b i t e d a maximum value at the onset of o s c i l l a t i o n and deformation of the drop. Johnson and B r a i d a ( l l ) observed c i r c u l a t i o n I n drops and drop o s c i l l a t i o n . They added a c o r r e c t i o n f o r 7 v i s c o s i t y of the continuous phase t o the Hu and KIntner (10) c o r r e l a t i o n , and separated the c o r r e l a t i o n curve i n t o regions of o s c i l l a t i n g drops and n o n - o s c i l l a t i n g drops. E l z i n g a and Banchero (12) found t h a t drag c o e f f i c i e n t s f o r drops cannot be r e l a t e d e n t i r e l y t o p h y s i c a l p r o p e r t i e s t h a t can be measured e a s i l y , because s m a l l q u a n t i t i e s of surface a c t i v e contaminants have a s i g n i f i c a n t e f f e c t . Trace q u a n t i t i e s of these contaminants may account f o r the di s c r e p a n c i e s between reported c o r r e l a t i o n s . Roger, T r i c e and Rushton (13) reported on the s i g -n i f i c a n t e f f e c t of surface contaminants on the s e t t l i n g time of d i s p e r s i o n s , and the presence of a p e a r l y grey f i l m at the i n t e r f a c e when these were present. J . T. Davies (14) reported on surface e f f e c t s and noted the la r g e e f f e c t of a s m a l l amount of surface a c t i v e i m p u r i t y on drop c i r c u l a t i o n , p a r t i c u l a r l y I n sm a l l s i z e d drops. Only one molecule aasorbed, per 1 0 5 A o 2 of drop surface would prevent c i r c u l a t i o n i n 0.01 cm. radius drops. He a l s o observed t h a t when an emulsion was being produced by shearing an o i l water mixture between two p l a t e s , the continuous phase of the emulsion tended t o be that which wetted the p l a t e s . 8 Buchanan ( 15) i n v e s t i g a t e d at d i f f e r e n t through-put v e l o c i t i e s the e f f e c t of the dispersed phase wetting and not wetting the o r i f i c e through which the d i s p e r s i o n was formed. I n a l l the aforementioned published l i t e r a t u r e s t u d i e s were l i m i t e d t o continuous flow of the dispersed phase through e i t h e r nozzles or o r i f i c e p l a t e s i n t o a c o u n t e r - c u r r e n t l y moving or i n t o a s t a t i o n a r y continuous phase. Not only have s e v e r a l drop s i z e d i s t r i b u t i o n s t u d i e s been r e p o r t e d , but a l s o seen i n most published photographs and o c c a s i o n a l l y mentioned, were s m a l l drops ( c a l l e d " t r a i l e r s " i n t h i s i n v e s t i g a t i o n ) which f o l l o w e d each main drop form. R o c c h i n i ( 16) i n h i s study of drop s i z e d i s t r i b u t i o n of methyl i s o b u t y l ketone dispersed through nozzles at 11 cm. per second i n a d i l u t e aqueous s o l u t i o n of a c e t i c a c i d , p l o t t e d frequency of occurrence against equivalent drop diameter and found two modes i n h i s frequency d i s t r i b u t l o n e c u r v e s . These modes presumably r e -presented drops and t r a i l e r s . The v e l o c i t y through the nozzle was w i t h i n the acceptable range suggested by K e i t h and Hl£s;onn ( 2 ) . Thus, except perhaps where flow r a t e s were very s m a l l and i n t e r f a c i a l t e n s i o n s r e l a t i v e l y l a r g e , i t would appear that d i s p e r s i o n s of t r u l y uniform drops were not produced. 9 Drop s i z e a f f e c t s I n t e r f a c i a l area, hold-up o f the dispe r s e d phase, mass t r a n s f e r c o e f f i c i e n t , and back-mixing ( 1 7 ) , which are the f o u r important f a c t o r s c o n t r o l l i n g the op e r a t i o n of l i q u i d - l i q u i d spray columns. I n t e r f a c i a l area i s i n -d i r e c t l y dependent upon drop s i z e and drop shape of the dis p e r s e d phase. Both the hold-up of the disp e r s e d phase and mass t r a n s f e r c o e f f i c i e n t are dependent upon the drop v e l o c i t y r e l a t i v e t o the continuous phase ( 1 8 ) . This v e l o c i t y i s i n t u r n a l s o a f u n c t i o n of drop s i z e . I t f o l l o w s t h a t s t u d i e s I n v o l v i n g the above f o u r important f a c t o r s would be g r e a t l y f a c i l i t a t e d i f a method could be obtained t o produce a l l the drops of a t r u l y uniform s i z e i n a l i q u i d - l i q u i d e x t r a c t i o n spray column. Sharkey ( 1 9 ) a p p l i e d a novel approach t o the produ c t i o n of t r u l y uniform drops by u s i n g a p e r i o d i c i n -j e c t i o n technique i n s t e a d of the continuous f l o w f o r m e r l y used. He i n j e c t e d a l i m i t e d q u a n t i t y of the disp e r s e d l i q u i d equal t o the volume o f a drop, by means of a mechanically d r i v e n s y r i n g e , which had t o be r e f i l l e d f o r each drop produced. Greene ( 2 0 ) Improved on t h i s by u s i n g a d i e s e l f u e l i n j e c t i o n pump which had an a b r u p t l y ended stroke and the advantages of ad j u s t a b l e speed, and a d j u s t a b l e volume per s t r o k e . He reported the formation of s i n g l e drops without t r a i l e r s at low nozzle throughput and low pump speed. The c h a r a c t e r i s t i c of t h i s pump was such t h a t where no t r a i l e r s were formed the drops would be of uniform s i z e . 10 I n view of the promising r e s u l t s reported by Greene, the purpose of t h i s present i n v e s t i g a t i o n was t o study the f e a s i b i l i t y of o b t a i n i n g t r u l y uniform drops,to reproduce the r e s u l t s of Greene, and t o study the e f f e c t s of nozzle diameter, nozzle v e l o c i t y time p r o f i l e , n ozzle m a t e r i a l , and of type of system on the p r o d u c t i o n A u n i f o r m s i z e drops. 11 EXPERIMENTAL INVESTIGATION I PRELIMINARY INVESTIGATION (A) Scope. The purpose of t h i s p a r t of the research was t o examine the f e a s i b i l i t y of o b t a i n i n g s i n g l e drops i n an n-butanol-water system and t o attempt t o reproduce the r e s u l t s obtained by Greene (20). He claimed t o have produced s i n g l e uniform drops without t r a i l e r s by pumping the n-butanol through a l / 8 i n . I . D. sharp edged s t a i n l e s s s t e e l nozzle i n t o water by means of a D i e s e l f u e l i n j e c t i o n pump coupled t o a Graham v a r i a b l e speed t r a n s m i s s i o n d r i v e n by a h.p. e l e c t r i c motor. The volume pumped per stroke was adjusted by p o s i t i o n i n g the a c c e l e r a t o r l i n k a g e w i t h brass shims of various gauge t h i c k n e s s . By p l o t t i n g mass throughput based on t o t a l shim t h i c k n e s s against pump speed based on speed t r a n s m i s s i o n d i a l s e t t i n g h e " p l o t t i n g regions of "no t r a i l e r s " , " t r a i l e r s w i t h some drops", "more than one t r a i l e r per drop", and "main drop s p l i t s . " (B) Apparatus. Figu r e 2 i s a photograph and f i g u r e 3 a diagrammatic layout of the apparatus used i n t h i s p a r t o f the I n v e s t i g a t i o n . The d i e s e l f u e l i n j e c t i o n pump, d r i v e and cam-actuated sw i t c h used by Greene are not shown i n f i g u r e 2 as t h i s part of the apparatus was mounted on the f l o o r t o avoid t r a n s m i t t i n g v i b r a t i o n t o the remainder of the apparatus mounted on the 12 FIGURE 2 Apparatus f o r the P r e l i m i n a r y I n v e s t i g a t i o n 13 A H U -x—I B I 1 o M A GENERAL LAYOUT * — 0 I 15" ELECTRIC COUNTER CIRCUIT S J ELECTRONIC FLASH CIRCUIT F I G U R E 3 DIAGRAMMATIC LAYOUT OF APPARATUS PRELIMINARY INVESTIGATION 14 TABLE 2 Key t o Figure 3 A 2000 ml. g l a s s storage b o t t l e B Screw clamp cock C Glass tee D 50 ml. b u r e t t e E D i e s e l f u e l i n j e c i t i o n pump F Graham v a r i a b l e speed [transmission and §• h.p. e l e c t r i c motor G Cam on d r i v e s h a f t t o actuate microswitches I and J H F i l l i n g f u n n e l f o r water phase I M i c r o s w i t c h t o actuate e l e c t r i c counter J M i c r o s w i t c h t o actuate e l e c t r o n i c f l a s h K A c c e l e r a t o r l i n k a g e rack end L Nozzle adapter and nozzle M " R o c c h i n i " square g l a s s column w i t h round l | i n . , column on top N Discharge storage 0 P r e s s u r i s i n g connection P Transformer Q E l e c t r i c counter R V a r i a b l e r e s i s t a n c e S Switch t o operate f l a s h c i r c u i t T Braun F60 e l e c t r o n i c f l a s h 15 l a b o r a t o r y bench. The di s p e r s e d phase, n-butanol flowed by g r a v i t y from an o u t l e t near the bottom of a 2,000 ml. storage b o t t l e A, through screw clamp cock B, t o g l a s s tee C. Connected t o t t h e upper s i d e of the tee C was a 50 ml. buret t e D vented back t o the top of storage b o t t l e A. The n-butanol flowed down through C t o the i n j e c t i o n pump mechanism. By i n j e c t i o n pump E i t was pumped through copper t u b i n g t o the nozzle L and Into the continuous water phase i n the square column M and the round column above. Here i t coalesced and flowed t o the used butanol storage v e s s e l N, a 1,000 ml. erlenmeyer f l a s k . The square column was b u i l t by Ro c c h i n i and described I n h i s t h e s i s (16). The cross s e c t i o n was square, the di s t a n c e between the opposite w a l l s being 1.5 i n . An e l e c t r i c counter Q powered by a transformer P w i t h a v a r i a b l e r e s i s t a n c e R i n s e r i e s f o r adjustment was actuated by a cam operated s w i t c h I mounted on the d r i v e s h a f t of the pump. T h i s counter counted pump r e v o l u t i o n s . i- The 50-ml. bu r e t t e was f i t t e d t o measure the volume of dispersed f l u i d pumped. By opening the screw clamp cock B, the bure t t e f i l l e d t o approximately the l e v e l of the f l u i d i n the storage b o t t l e A. Then by c l o s i n g cock B, the f l u i d pumped was made t o come only from the b u r e t t e . By measuring the time i n t e r v a l , the number of r e v o l u t i o n s 16 and the volume run from the burette, both volume per stroke and revolutions per second of the pump were obtained. The o p t i c a l system was .-.arranged so that the drops i n the column would be photographed simultaneously i n .two directions at r i g h t angles. By t h i s arrangement a l l three axes of each drop were obtained i n the same photograph. Figure 4 shows the o p t i c a l system used f o r the preliminary i n v e s t i g a t i o n . A v e r t i c a l s l o t 1§- i n . wide was cut i n the v e r t i c a l supporting panel behind the column. A wooden box Y containing a Braun F60 e l e c t r o n i c f l a s h T at the back and a ground glass d i f f u s e r X at the front, was screwed to the back of the panel of the apparatus behind the l | - i n . wide v e r t i c a l s l o t . A t r a c i n g paper r e f l e c t o r and d i f f u s i n g screen V provided even i l l u m i n a t i o n at the back of the column. To improve contrast a dark background was provided d i r e c t l y behind the drops by f i x i n g two v e r t i c a l 3 / 8 i n . wide opaque s t r i p s (W) at the v e r t i c a l center l i n e s of the rear faces of the column. Maximum contrast Is very necessary when photographing n-butanol drops In water as the difference i n r e f r a c t i v e Indices i s very small. The two adjustable mirrors U and the two f i x e d mirrors Z enabled the camera, a 35-mra« r e f l e x Exakta I l a with Biotar lens 2 / 5 8 f i t t e d with extension tubes, to photograph the drops In two perpendicular directions at the one time. 17 The o p t i c a l system was adjusted by r o t a t i n g and moving the adj u s t a b l e m i r r o r s U u n t i l the nozzle t i p not only appeared d i r e c t l y i n f r o n t of the .dark s t r i p ¥ I n each view, but a l s o was i n focus i n each view when observed through the v i e w f i n d e r of the camera. (C) Procedure. Examination of the i n j e c t i o n pump E f i g u r e 3 showed t h a t a considerable amount of i n t e r n a l c o r r o s i o n had taken p l a c e . The i n j e c t o r was r e p l a c e d , and a l l p a r t s exposed t o 1 the pumped f l u i d were thoroughly washed out w i t h f i r s t acetone and then w i t h n-butanol. The storage b o t t l e A was.charged w i t h t e c h n i c a l grade n-butanol, as used by Greene, and the column f i l l e d w i t h d i s t i l l e d water. The brass spacer system (20) f o r " t h r o t t l e " a d j u s t -ment on the pump was found t o be u n s a t i s f a c t o r y ; as i t provided a much too coarse adjustment. Even the t h i c k n e s s ? o f a piece of paper made a considerable d i f f e r e n c e t o the volume pumped. I n view of t h i s , a very simple screw adjustment was provided, and the backlash i n the r a c k - p i n i o n l i n k a g e was removed by packing out the rack and s p r i n g - l o a d i n g the rack l o n g i t u d i n a l l y . 18 I CAMERA F I G U R E 4 OPTICAL ARRANGEMENT PRELIMINARY INVESTIGATION SCALE' 3" = r-0,r 18 TABLE 3 Key t o Fig u r e 4 T Braun F 6 0 e l e c t r o n i c f l a s h U '• Adjustable m i r r o r s s i l v e r e d on the f r o n t s i d e V T r a c i n g paper d i f f u s e r W 3/Q i n . v e r t i c a l opaque s t r i p X Ground o p a l gjLass Y Wood box w i t h l i d housing e l e c t r o n i c f l a s h and o p a l g l a s s screen Z F i x e d m i r r o r s s i l v e r e d on the f r o n t s i d e . 19 To reduce the a i r leakage i n t o the system a 6 f t . water head of a i r pressure was a p p l i e d t o the system at 0 ( f i g u r e 3). Although t h i s e l i m i n a t e d a i r leakage at low speeds, i t f a i l e d t o do so at hi g h speeds and h i g h d e l i v e r i e s . Once a i r leaked i n t o the system, the r e s u l t i n g f l u i d , n - b u t a n o l and a i r mixture,was compressible, and the e f f e c t of the r a p i d i n j e c t i o n and shut o f f was l o s t . S e v e r a l t e s t runs then were made t o f i n d the best o p t i c a l system. The best p o s i t i o n s of the e l e c t r o n i c f l a s h T and d l f f u s e r g l a s ses X are shown i n f i g u r e 4. The best negatives were obtained w i t h camera lens aperture s e t t i n g f . l 6 , Kodak High Contrast P o s i t i v e f i l m , t e n minute development of the f i l m i n Kodak D - l l developer at 70°F, and f i x i n g w i t h Kodak F-5 F i x e r . To take a photograph, the camera s h u t t e r set at Bulb was opened and swi t c h S ( f i g u r e 3) c l o s e d manually. As soon as the cam G on the pump d r i v e s h a f t c l o s e d the microswitch J and completed the c i r c u i t , t h e f l a s h was f i r e d . The s h u t t e r was then r e l e a s e d and sw i t c h S opened. Sy n c h r o n i z a t i o n of t h i s l/lOOO second f l a s h w i t h a s p e c i f i c p a r t of the drop formation c y c l e was adjusted by r o t a t i n g the cam G r e l a t i v e t o the s h a f t . , 20 Eleven runs were made u s i n g Greenes 1/8 I n . I.D. s t a i n l e s s s t e e l nozzle ( 2 0 ) , I n which s e l e c t e d pump speeds ranged from 6 t o 1.67 s t r o k e s per second, and the volume per stroke v a r i e d from 0 t o (a maximum of ) 0 .020 ml. f o r each s e l e c t e d pump speed. I n none of these runs were c o n s i s t a n t s i n g l e drops without t r a i l e r s observed. Even when v i s u a l i n s p e c t i o n through the column f a i l e d t o i d e n t i f y the presence of t r a i l e r s , p r o j e c t i o n on a screen of the photograph negatives i n v a r i a b l y showed the presence of one or more t r a i l e r s per drop. A 5/32 i n . I.D. s t a i n l e s s s t e e l nozzle was made, f o l l o w i n g thecidesign of Greene's 1/8 i n . s t a i n l e s s s t e e l nozzle except f o r the i n s i d e diameter. Runs 12 and .13 were Soiisecutive made w i t h t h i s n o z z l e , and up t o e l g n t A s i n g I e drops without t r a i l e r s were produced at a drop s i z e of 0.005 ml. and a frequency of I . 6 5 t o I . 8 5 strokes per second. As a r e s u l t of these promising r e s u l t s w i t h the 5/32 i n . I.D. s t a i n l e s s s t e e l n o z z l e , I t was decided t o continue t h i s i n v e s t i g a t i o n w i t h a more v e r s a t i l e pump where the v e l o c i t y p r o f i l e of the discharge could be v a r i e d , and w i t h the apparatus modified by improving the p i p i n g and the o p t i c a l systems. 21 I I MAIN INVESTIGATION (A) SCOPE The main i n v e s t i g a t i o n was planned t o study the e f f e c t of a number of f a c t o r s on the r e g i o n of s i n g l e drops obtained i n p l o t s of drop volume against the number of pump strokes per second. These f a c t o r s under study were nozz l e s i z e , nozzle m a t e r i a l , v e l o c i t y - t i m e p r o f i l e of d i s p e r s e d phase flow through the nozzle at drop formation, pump strokes per second and the p a r t i c u l a r system used. The nozzle s i z e s t o be examined,were t o be those that produced s i n g l e drops most e a s i l y . The nozzle m a t e r i a l s used were s t a i n l e s s s t e e l Type 316, b r a s s , and T e f l o n . Due t o d i f f i c u l t y experienced by the workshop i n manufacturing s a t i s f a c t o r y sharp edged s t a i n l e s s s t e e l n o z z l e s , brass n o z z l e s were us«d !.for the main part of t h i s i n v e s t i g a t i o n . The bore could not be made s t r a i g h t f o r the whole l e n g t h of the s t a i n l e s s s t e e l n o z z l e s . These nozzles were t h e r e f o r e d r i l l e d from each end r e s u l t i n g i n a step midway down the n o z z l e . Two runs were made w i t h a T e f l o n n o z z l e , T e f l o n being chosen as a m a t e r i a l t h a t would not be wet by the water phase. The d e s i r e d types of v e l o c i t y - t i m e p r o f i l e s appeared t o be most e a s i l y obtained by u s i n g a cam operated p o s i t i v e displacement pump, where the f l o w was d i r e c t l y r e l a t e d t o the cam p r o f i l e . 22 (B) MODIFICATIONS TO EXISTING APPARATUS. ( i ) Design of pump and c a l i b r a t i o n . As the d i e s e l i n j e c t i o n pump was u n s u i t a b l e f o r adaption t o the use of d i f f e r e n t cams, and as the i n j e c t o r design d i d not permit the pr e v e n t i o n of a i r leakage i n t o the system, t h i s pump was abandoned. A Hoke 1/8 i n c h bellows s e a l needle valve ( f i g u r e 5) was examined f o r a d a p t a t i o n t o use as a bellows pump. By u s i n g a bellows as the pump no leakage of a i r was p o s s i b l e , and by compressing the bellows w i t h a plunger i n s t e a d of the screw cap, a p o s i t i v e displacement pump r e s u l t e d . •• . , . The c h a r a c t e r i s t i c s of t h i s v alve used as a pump ( f i g u r e 6) were t e s t e d , t o see i f the volume pumped v a r i e d d i r e c t l y w i t h the s t r o k e , and t o see i f the maximum volume pumped was adequate. A c a p i l l a r y tube, assumed t o be of j constant cross s e c t i o n , was c a l i b r a t e d i n ml. per i n c h of le n g t h by f i l l i n g 25 i n . of i t w i t h water, a l l o w i n g the water t o run i n t o a 25 ml. graduated c y l i n d e r . This procedure was f o l -3i0w&d f o r a t o t a l of f o u r times. By d i v i d i n g the t o t a l volume by 100, the c a p a c i t y per u n i t l e n g t h of c a p i l l a r y t u b i n g was,determined. 23 A Valve bellows s e a l B Cap thread C Valve discharge D Valve i n l e t E Valve cap Hoke 1/8 i n FIGURE 5 bellows s e a l needle valve 24 F Hoke bellows valve G Cap thread of valve H Valve holder (Figure 7) I Machine screws FIGURE 6 Bellows valve pump 25 The c a p i l l a r y was connected t o the valve "by means of an I m p e r i a l i n . tube x l / 8 female I.P.S. compression adapter. A f e r r u l e made from T e f l o n tape was used. The b e l -lows valve and part of the c a p i l l a r y tube were f i l l e d w i t h water and a piece of graph paper 10 d i v i s i o n s x 10 d i v i s i o n s t o the §• i n c h placed behind the tube so t h a t the di s t a n c e of any movement along the tube could be estimated t o 0.01m. By screwing down the cap (compressingtthe bellows s e a l ) f i g u r e 5* the water was f o r c e d up the c a p i l l a r y tube. The dist a n c e the meniscus t r a v e l l e d at the end of each quarter t u r n was noted, and i s shown i n t a b l e 4. From t h i s c a l i b r a t i o n t e s t the average discharge per quarter t u r n was 0.204 i n . of c a p i l l i a r y , and the maximum d e v i a t i o n from t h i s mean between §• and 1§ tur n s was l e s s than 10$. The average change i n volume of the bellows f o r a compression of 0.01 inches was found t o be 0.0088$ ml. Therefore, f o r the estimated maximum compression of the bellows of l / l 6 i n . the volume pumped was 0.056 ml. As the maximum volume of n-butanol pumped per stroke i n the p r e l i m i n a r y i n v e s t i g a t i o n was 0.020 ml., the volume pumped by t h i s bellows s e a l v a l v e pump was considered adequate f o r the n-butanol water system. 26 TABLE NG. 4 CALIBRATION OF 1/8 i n . HOKE BELLOWS SEAL VALVE #432 FOR CHANGE IN VOLUME PER STROKE DISTANCE (a) C a l i b r a t i o n of measuring c a p i l l a r y tube assumed t o be of uniform c r o s s - s e c t i o n . Volume measured f o r 100 i n . l e n g t h = 4 .5-ml. Volume per 1 i n . l e n g t h = 0.o4'5-ml. (b) C a l i b r a t i o n of bellows s e a l v a l v e . T o t a l . of turns cap. Reading on graphnpaper s c a l e inches Change of height inches e 0.9 i i+ 1.15 0 .25 i 2 1.35 0.20 3/4 1.55 0.20 1 1.75 0.20 1.97 0.22 H 2 .17 0.20 Volume P i t c h per r e v o l u t i o n of cap. = of thread = (0.82) (0.045) ml. 0.0369 ml. 1/24 i n . Volume per 0.01 i n . advance = 0.00886 ml. The readings f o r the 0 and \ t o t a l t urns of the cap were neglected t o avoid any back l a s h e r r o r . 27'/' Two check valves were made by d r i l l i n g 5/32 i n . diameter holes h a l f way through two 1/8 i n . I.P.S. x 3/16 i n . t u b i n g f l a r e d h a l f unions I m p e r i a l 48P. I n one the hole was d r i l l e d from the thread end and i n the other from the f l a r e d end. A 1/8 i n . s t e e l b a l l b earing was tappedcinto the bottom of each of these holes t o produce a s p h e r i c a l l y shaped seat i n place of the cone from the d r i l l i n g o p e r a t i o n . A 1/8 i n . s t a i n l e s s s t e e l b a l l b e a r i n g was then dropped i n t o the hole t o repla c e the s t e e l b a l l , and a s m a l l keeper f o r c e d i n at the top t o a l l o w the b a l l about 1/32 i n . movement but not permit i t t o come out of the adapter. Although these check val v e s c l o s e d by g r a v i t y they were more p o s i t i v e i n a c t i o n than spring-loaded commercial u n i t s . The Hoke valve was then made i n t o a bellows pump by a t t a c h i n g w i t h appropriate f i t t i n g s two check val v e s t o each of the discharge and the s u c t i o n ends. At each end one check valve was an I m p e r i a l No. 6 3 P and the other made by the author. The Hoke valve was arranged so tha t the opening i n the valve t o the bellows was on the discharge s i d e . ( i i ) Pump mechanism. The bellows valve was then screwed i n t o a ho l d e r ( f i g u r e s 6 and 7) which, i n t u r n , was screwed t o a cam-operated a d j u s t a b l e - s t r o k e mechanism, modified from the apparatus used by Thomson ( 2 1 ) . A plunger rod cap a l s o 28 shown i n f i g u r e 7 was f i t t e d t o the rod of the stroke arm, and pressed against the top of the bellows v a l v e . Figure 8 shows the cam-operated a d j u s t a b l e -stroke mechanism. Cam A operated the modified cam f o l l o w e r B ( f i g u r e s 8 and 9) by p r e s s i n g against a f o l l o w e r wheel,a 3/8 i n . p r e c i s i o n Departure R2 b e a r i n g , f i t t e d on the bearing post ( f i g u r e 7) mounted i n the f o l l o w e r . The cam f o l l o w e r B ( f i g u r e 8) operated the v e r t i c a l r a t i o l e v e r C about the movable fulcrum D c o n t r o l l e d by the knurled knob E. The v e r t i c a l r a t i o l e v e r C, o s c i l l a t i n g about fulcrum D, actuated the stroke arm F which i n t u r n operated the pump. By t u r n i n g knurled knob E, the fulcrum was moved up or down changing the r a t i o between the motions of the cam f o l l o w e r and the stroke arm. The volume pumped per stroke f o r a given cam was c o n t r o l l e d by a d j u s t i n g knob E which p o s i t i o n e d the movable fulcrum D. The v e l o c i t y p r o f i l e of the stroke arm F was c o n t r o l l e d by the cam p r o f i l e , cam speed, and p o s i t i o n of movable fulcrum D. ( i i i ) Cams. Two cams were designed ( f i g u r e 11) and made t o provide the pump discharge stroke w i t h the f o l l o w i n g motions: (a) Cam A ( f i g u r e 10) r o t a t i n g i n forward d i r e c t i o n (counter-clockwise) produced uniform a c c e l e r a t i o n , then constant v e l o c i t y and f i n i s h e d w i t h a sudden stop. This motion w i l l be c a l l e d Cam "A" forward. (-5 T 44- £ I—KvJ L. js*-l_ight press fit with T'22l~\ |-'Departure R 2 ball bearing used as a follower wheel. B E A R I N G P O S T S c a l e : Twice Size l~No. 50 Drill, 2-56 U N C - 2 B R O D C A P Scale Twice Size 5. Drill x i deep 16 4 ^ - 28 UN - 2B §zDfi\l 2 holes V A L V E H O L D E R S c a l e . Full Size F I G U R E 7  P U M P D R I V E C O M P O N E N T S S C A L E S AS SHOWN FIGURE 8 Cam operated a d j u s t a b l e - s t r o k e mechanism 331 TABLE NO. 5 Key t o Figu r e 8 CAM OPERATED ADJUSTABLE-STROKE MECHANISM A Cam B Modif i e d Cam Fol l o w e r ( f i g u r e 7) C V e r t i c a l R a t i o Lever D Movable Fulcrum E Knurled C o n t r o l Knob F Stroke Arm G Valve Holder it-"rnr JJ=UL I 2 _1 - | c M 1 -|00 -|OB 4 t3 8 0 2000 02003 win R N ° 50 D r i l l , 2 - 56 UNC - 2B 2^ ^4 . 3 , 16 3 8 Drill ft Tap for existing post-I R 16 A Drill N° 50 Dr i l l , 2- 56 UNC-2B F I G U R E 9 CAM FOLLOWER S C A L E * T W I C C S I Z E » 34 Cam " A " F o r w a r d r o t a t i o n ) R e v e r s e r o t a t i o n } FIGURE 11 Cams " A " and "B (b) Cam A r o t a t i n g i n the reverse d i r e c t i o n ( clockwise) produced uniform a c c e l e r a t i o n , then constant v e l o c i t y and f i n i s h e d w i t h uniform d e c e l e r a t i o n . T h i s motion w i l l be c a l l e d Cam "A" reversed. , (c) Cam B i n e i t h e r d i r e c t i o n produced simple harmonic motion. This motion w i l l be c a l l e d Cam "B". Figure 10 shows the design of cam A and the cam diagram. The cam f o l l o w e r (and stroke arm) were a c c e l e r a t e d from 0°-3O° r o t a t i o n , kept at constant v e l o c i t y from 30°-90° and then suddenly stopped at 90°. From 90° t o 150° the f o l l o w e r and stroke arm were at r e s t . The f o l l o w e r and stroke arm were a c c e l e r a t e d u n i f o r m l y i n the negative d i r e c t i o n from 150°-180°, kept at uniform v e l o c i t y from l80°-240°, and decelerated u n i f o r m l y t o r e s t from 240° - 2 7 0 ° . From 270°-360°, the f o l l o w e r was at r e s t . To f a c i l i t a t e the manufacture of the cam and enable\ i t t o be made i n the Department workshop, " m i l l i n g machine c u t t e r " t r a v e l d i s t a n c e from maximum ra d i u s of the cam f o r each 2° of r o t a t i o n was t a b u l a t e d . The cam could then be set up 4n a r p t a t i n g head of the m i l l i n g machine, r o t a t e d 2°from the maximum r a d i u s p o s i t i o n , and the c u t t e r f e d i n t o the cam up t o the t a b u l a t e d c u t t e r t r a v e l d i s t a n c e . The cam was r o t a t e d a f u r t h e r 2°, and phe c u t t e r f e d t o the next t a b u l a t e d t r a v e l d i s t a n c e . This was repeated u n t i l the minimum r a d i u s 36 was reached. To avoid backlash the cam was always r o t a t e d i n the d i r e c t i o n of reducing r a d i u s . The cam was l i g h t l y rubbed w i t h f i n e emery paper t o remove the d i s c o n t i n u i t y humps. The cam p r o f i l e was checked by assembling the cam i n the. cam operated a d j u s t a b l e stroke mechanism ( f i g u r e 8). A d i a l gauge reading d i r e c t l y t o 0.0005 i n . and estimated t o 0.0001 in.was placed at the end of the stroke arm t o measure the stroke arm t r a v e l . Knob E was adjusted u n t i l a change i n d i a l reading of 0.025 i n . was obtained per cam r e v o l u t i o n . As the maximum designed cam f o l l o w e r t r a v e l was 01250 i n . f o r cam A, the r a t i o of cam f o l l w e r t r a v e l t o stroke arm t r a v e l was 10:1. Consequently the cam f o l l o w e r t r a v e l was measured w i t h a p r e c i s i o n 0.001 i n . While the apparatus was run at a s u i t a b l e speed, the d i a l gauge was photographed w i t h the Bolex 16H R e f l e x movie camera at 64 frames per second. By p l o t t i n g the readings against frame numbers the a c t u a l cam p r o f H e was obtained. I t was determined t h a t I.635 0 of r o t a t i o n occurred per camera frame. TJie maximum d e v i a t i o n from the designed p r o f i l e was found, t o be 0.005 i n . The cam B was designed t o give simple harmonic motion and t h e r e f o r e was simply an e c c e n t r i c d i s c centered 1/8 i n . from the shaft centre l i n e . The d u r a t i o n of the discharge stroke f o r cam B was t h e r e f o r e 180° of r o t a t i o n , 37 whereas f o r cam A forward' i t was 90° of r o t a t i o n , and f o r cam A re v e r s e d i t was 120 of rotation'. ( i v ) P i p i n g m o d i f i c a t i o n s . Considerable m o d i f i c a t i o n was made t o the p i p i n g of the apparatus, based on both the experience gained from the p r e l i m i n a r y i n v e s t i g a t i o n and the proposed future use of methyl i s o b u t y l " ketone. The 50-ml. b u i e t t e was rep l a c e d by a 5-ml. b u r e t t e to enable volumes to be measured w i t h greater" p r e c i s i o n . A l l neoprene tubing except f o r the vent from the b u r e t t e D ( f i g u r e 12) to the 2000 ml. storage b o t t l e £: was r e p l a c e d by copper t u b i n g . "Kovar"' g l a s s to copper adapters were used at the o u t l e t of the storage b o t t l e A and the burette.- The screw clamp cock between the storage b o t t l e . A and the burette was replaced by a 1/8 in.. Hoke #**32 bellows s e a l v a l v e C. A s t a i n l e s s s t e e l a i r t r a p E adapted from a constant head tank was i n s t a l l e d i n the Une between the burette D and the pump, to prevent any a i r entering the pumping system. This a i r t r a p was vented through a 1/8- i n . Hoke #*32 bellows s e a l valve F. Cv) O p t i c a l modifications... •ks the photographic r e s u l t s from the p r e l i m i n a r y i n v e s t i g a t i o n were ve r y disappointing,., a more thorough examination of the o p t i c a l system was made... Also i n view of the intended use of a Bolex Hl6 R e f l e x movie camera w i t h a Ly t a r S.O . M . B e r t h i o t l e n s 1.8/25, the use of the e l e c t r o n i c f l a s h was un s u i t a b l e . 38 A 16 i n . x 12 i n . F r e s n e l lens a v a i l a b l e i n the Department was mounted i n a i i n . p l y wood box. The back end was f i t t e d w i t h a 2 i n . tube through wich an automobile head lamp, mounted i n a 2 i n . diameter h o l d e r , could be moved i n and out, enabling the fi l a m e n t of the lamp t o be placed i n f r o n t o f , a t , or behind the focus of the l e n s . By having the fi l a m e n t at the focus, a very poor background appeared behind the drops, but by p l a c i n g a 60 watt f r o s t e d bulb at the back of the tube i n l i e u of the automobile head lamp, not only d i d a reasonably c o l l l m a t e d beam of l i g h t appear, but a l s o a good even background f o r the drops r e s u l t e d . By u s i n g an auto-transformer any d e s i r e d l i g h t i n t e n s i t y was obtained. Due t o both the imp e r f e c t i o n s of the l e n s , and the f a c t t h a t there was no chromatic c o r r e c t i o n , monochromatic l i g h t obtained by p l a c i n g r ed cellophane over the l | i n . s l i t behind the column ( f i g u r e s 12 and 14) g r e a t l y improved image sharpness. Figure 14 shows the o p t i c a l layout used f o r t h i s part of the resea r c h . The c o l l l m a t e d beam of l i g h t passed through the red cellophane, then through the s l i t B t o the r e a r f i x e d m i r r o r s C mounted at r i g h t angles t o one another on the column. These m i r r o r s s p l i t the beam i n t o two halves; each, a f t e r being r e f l e c t e d from the r e a r a d j u s t a b l e mounted Front Rear FIGURE 12 Apparatus 40 TABLE 6 Key t o Figu r e 12 A Storage b o t t l e B E l e c t r i c counter C Hoke valve r e p l a c i n g former screw clamp cock D 5-ral» measuring b u r e t t e E A i r t r a p F Hoke v a l v e , vent t o a i r t r a p G Outlet valve of a i r t r a p H Nozzle l i n e 41 FIGURE 13 Mounted F r e s n e l Lens 4 2 m i r r o r s D, passed through the square column normal t o the r e a r f a c e s . The f r o n t a d j u s t a b l e m i r r o r s E r e f l e c t e d these beams t o the f r o n t f i x e d m i r r o r s F (mounted at 70° t o one another) where the two beams were r e f l e c t e d t o the s t i l l o r movie camera and focused on the f i l m . This system provided very good c o n t r a s t , and as a r e s u l t Kodak Plus X Pan f i l m was used f o r s t i l l p i c t u r e s i n l i e u of the Kodak High Contrast P o s i t i v e so t h a t i t might be as n e a r l y s i m i l a r as p o s s i b l e t o the 16 mm f i l m Eastman Plus X r e v e r s a l f i l m a v a i l a b l e f o r the movie camera. I n order t o make the o p t i c a l system more r i g i d , the square column and p o r t a b l e m i r r o r holders ( f i g u r e 1 5 ) f o r the « - -a d j u s t a b l e f r o n t and r e a r m i r r o r s were fastened w i t h screws t o a 1/16 i n . brass p l a t e which was r i g i d l y mounted one i n . above the h o r i z o n t a l s h e l f of the apparatus. Supports f o r both the Bolex 16H R e f l e x camera and the Exakta camera were modified t o a l l o w f o r t h i s a d d i t i o n a l height of the column. The adjustment and alignment of the f r o n t s i l v e r e d m i r r o r s and F r e s n e l lens were c a r r i e d out as f o l l o w s : each r e a r a d j u s t a b l e m i r r o r D ( f i g u r e 14) was r o t a t e d and moved i n and out u n t i l , viewed through the appropriate f r o n t face of the square column along a l i n e p e r p e n d i c u l a r t o the face and passing through the n o z z l e , the widest and b r i g h t e s t s t r i p of l i g h t appeared centred behind the n o z z l e . The r e a r 1 S C A L E : 1/2 SIZE F I G U R E 14 REVISED MIRROR ARRANGEMENT 44 ^ Drill, csk. for No. 4screw 2 holes -'..-,1 . 4 HOLDER BASE No. 36 Drill No. 6-32UNe-2B r 3 _ 8 - |CM Ploce | - I 6 U N C - 2 B nut a washer on post before soldering top. 3 -Solder | - I 6 U N C - 2 A -o —I CM MIRROR HOLDER i" 16 Brass T rowo H O L D E R S T R I P OJ FIGURE 15 PORTABLE MIRROR HOLDERS S C A L E : F U L L S I Z E 45 a d j u s t a b l e m i r r o r s were next placed i n the m i r r o r holders and r o t a t e d and moved i n and out u n t i l two views of the nozzle appeared d i r e c t l y i n f r o n t of the b r i g h t bands and were both i n focus when observed i n the view f i n d e r of the Exakta camera w i t h f . 2 lens aperture s e t t i n g . R o t a t i n g the f r o n t a d j u s t a b l e m i r r o r s moved the two Images together or apart and a l s o the views of the nozzles i n r e l a t i o n t o the b r i g h t background bands. Moving the m i r r o r s away from the column incre a s e d the object d i s t a n c e but moved the images towards one another. I n order t o have a s u i t a b l e d i s t a n c e of focus f o r a s a t i s f a c t o r y image s i z e i t was found t h a t by having the f r o n t f i x e d m i r r o r s if at 90° w i t h one another, the photograph images were at the ex-treme outsides of the frame. By reducing t h i s i n c l u d e d angle t o 70° the images were adjacent t o one another. With t h i s arrangement 2.5 cm. extension tubes were used w i t h the Exakta camera and a l / l 6 I n . shim under the lens of the Bolex H16 R e f l e x camera. The F r e s n e l lens ( f i g u r e s 13 and 16) was next l o c a t e d f o r both cameras by f i r s t s e t t i n g the Exakta camera aperture at f . l 6 and then a d j u s t i n g the l o c a t i o n of the F r e s n e l lens u n t i l an evenly d i v i d e d and b r i g h t background appeared i n the v i e w f i n d e r . The aperture was then opened t o f . 2 , and s h u t t e r speed set at 1/1000 sec. 4 6 FIGURE 1 6 Apparatus set up w i t h Bolex H 1 6 Reflex Camera 47 A 60 v o l t s e t t i n g w i t h the auto-transformer provided the c o r r e c t l i g h t i n t e n s i t y f o r Kodak Plus X Pan w i t h the camera set a f.2 and 1/1000 sec. when the m i r r o r s were b r i g h t and new. S i m i l a r l y a 40 v o l t s e t t i n g provided the c o r r e c t l i g h t i n t e n s i t y f o r Eastman Plus X r e v e r s a l f i l m w i t h the Bolex camera set a f . 1.8, 64 f. p . s . , and,shutter one quarter open (equivalent of an exposure time of 1/640 s e c ) . As the f r o n t s i l v e r e d m i r r o r s t a r n i s h e d these voltages had t o be incre a s e d . 48 (C) EXPERIMENTAL WORK WITH THE N-BUTANOL AND WATER SYSTEM ( i ) Charging the apparatus. • A f t e r the m o d i f i c a t i o n s had been completed a l l the equipment i n contact w i t h the n-butanol was washed out w i t h acetone and then water. The p i p i n g was disconnected at the bottom of the a i r t r a p E ( f i g u r e 12) and the l i n e s and pump removed and blown out w i t h a i r . The p i p i n g then was r e -connected t o the bottom of the a i r t r a p , and the nozzle l i n e H connected t o a vacuum pump. A l l valves were c l o s e d and the storage b o t t l e A ( f i g u r e 12) f i l l e d w i t h water saturated t e c h n i c a l grade n-butanol. Valve C was opened, and then F opened u n t i l N-butanol flowed out of the vent from the a i r t r a p E. Valve P was then c l o s e d . The vacuum pump then was s t a r t e d and a f t e r maximum vacuum was reached a very s m a l l amount of n-butanol was allowed t o pass through "G". A f t e r the vacuum was again at a maximum the process was repeated. The rubber l i n e t o the vacuum pump from the copper nozzle l i n e was clamped and then valve G opened, a l l o w i n g the n-butanol t o f i l l the evacuated bellows pump and l i n e . The vacuum pump next was removed and the nozzle adapter and 1/8 i n . s t a i n l e s s s t e e l nozzle assembled i n the column. The column then was f i l l e d w i t h d i s t i l l e d water. The reason f o r the evacuation was t o remove any a i r from the Insi d e of the bellows. This procedure proved very s u c c e s s f u l . 49 ( i i ) E x a m i n a t i o n o f drops pr o d u c e d w i t h s t a i n l e s s . s t e e l n o z z l e s . A d e t a i l e d s t u d y o f drops formed w i t h s t a i n l e s s s t e e l n o z z l e s was made u s i n g t h e f o l l o w i n g p r o c e d u r e : (a) f The Graham V a r i a b l e Speed T r a n s m i s s i o n was s e t a t a s e l e c t e d v a l u e . (b) The volume p e r s t r o k e o f t h e pump was r e g u l a t e d by a d j u s t i n g knob E ( f i g u r e 8) o f t h e cam o p e r a t e d a d j u s t a b l e s t r o k e mechanism u n t i l a minimum v a l u e was o b t a i n e d f o r t h e d e s i r e d drop c o m b i n a t i o n (one drop and z e r o t r a i l e r , one drop and one t r a i l e r e t c . ) . As t h e i n v e s t i g a t i o n was c a r r i e d out i n t h e d i r e c t i o n o f i n c r e a s i n g volume p e r s t r o k e f o r each s e l e c t e d v a l u e i n ( a ) , t h e v a l u e s o b t a i n e d r e p r e s e n t e d f i r s t change i n t o t h e p a r t i c u l a r drop c o m b i n a t i o n under s t u d y . O b s e r v a t i o n o f t h e drops b e i n g formed was b e s t made by l o o k i n g t h r o u g h t h e v i e w f i n d e r o f t h e E x a k t a camera w i t h t h e f o c u s s i n g m a g n i f i e r i n p l a c e . (c ) V a l v e C f i g u r e 12) was c l o s e d , and when t h e meniscus pass e d t h e z e r o mark on t h e b u r e t t e D, b o t h t h e e l e c t r i c c o u n t e r was r e a d and t h e c l o c k s t a r t e d . A f t e r a s u i t a b l e i n t e r v a l o f t i m e , s i m u l t a n e o u s l y t h e c l o c k was sto p p e d and t h e b u r e t t e and t h e c o u n t e r r e a d . The t i m e i n seconds, t h e volume pumped i n m i l l i l i t r e s and t h e d i f f e r e n c e i n 50 r e v o l u t i o n s were recorded. Valve C was then opened, a l l o w i n g the bure t t e t o r e f i l l . (d) During the time i n t e r v a l i n ( c ) , s t i l l photographs were taken w i t h the Exakta camera so as t o have a permanent r e c o r d . (e) Procedures(b) and (c) were repeated f o r each drop combination at each s e l e c t e d speed i n ( a ) . By d i v i d i n g the number of r e v o l u t i o n s i n t o the volume pumped, and the time i n seconds i n t o the number of r e v o l u t i o n s , the volume per stroke and the number of pump strokes per second were obtained. To determine the boundaries of the var i o u s areas of drop combinations obtained i n graphs w i t h volume per stroke as o r d i n a t e , and pump strok e s per second as a b s i s s a , the above minimum values were p l o t t e d . As the main pur-pose of t h i s i n v e s t i g a t i o n was the study of uniform s i z e d drops without t r a i l e r s , i n regions where t h i s drop com-b i n a t i o n e x i s t e d , both the upper and the lower boundaries and sometimes, i n a d d i t i o n , intermediate p o i n t s were what was determined. In runs 14 t o 24 some 300 observations of drop c h a r a c t e r i s t i c s and number of t r a i l e r s were made i n a range of drop volume from approximately 6.0 x 10"^ t o 33 x 10"^ ml. and of pump speed from 0 t o 4.33 strokes per second, u s i n g n-butanol and water system w i t h mutually s a t u r a t e d phases, 51 a 1/8 i n . I.D. nozzle and Cam A forward. Figure 17 shows the types of drops produced up to a pump speed of approximately 2 .5 strokes per second. Nowhere during these observations were any s i n g l e drops w i t h -out t r a i l e r s found. The l i n e marked "bounce" i n d i c a t e s the lower l i m i t of the r e g i o n where the sm a l l t r a i l e r f o l l o w i n g each l a r g e r drop, i s a c c e l e r a t e d part way up the column, s t r i k e s the bottom of the main drop and bounces o f f t o one s i d e . This phenomena was reported by Buchanan (15)« The t r a n s i t i o n between the formation of m u l t i p l e drops and drops w i t h t r a i l e r s was qu i t e sharp at 0.48 strokes per second. As no s i n g l e drops without t r a i l e r s were observed duri n g the examination of drop formation w i t h the 1/8 i n . I.D. s t a i n l e s s s t e e l n o z z l e , t h i s n ozzle was replaced by the 5/32 i n . I.D. s t a i n l e s s s t e e l n o z z l e , and the column r e f i l l e d w i t h d i s t i l l e d water. Then the bellows valve pump was operated d i s p e r s i n g the n-butanol i n t o the water u n t i l the c o n c e n t r a t i o n t r a i l s behind each drop ceased t o be formed. The water then was assumed t o be saturated w i t h the n-butanol. P o r t a b l e spacer pieces of 1/4, 5/l6 and 3/8 i n . t h i c k n e s s were made f o r f i t t i n g over the cam f o l l o w e r guide. These l i m i t e d the t r a v e l of the cam f o l l o w e r B ( f i g u r e 8) so that the f o l l o w e r wheel contacted only t h a t p o r t i o n of the L E G E N D MINIMUM VALUES FOR g I DROP 8 I TRAILER 6 I. DROP & 2 TRAILERS O I DROP a 3 TRAILERS O BOUNCE DROP S I LARGE TRAILER 9 9-0-50 100 PUMP STROKES 7 SEC. FIGURE 17 RUNS 14-24 TYPES OF DROPS PRODUCED !/8!! STAINLESS STEEL NOZZLE CAM MA" FORWARD n - B U T A N O L and WATER 2-00 53 cam of l a r g e r r a d i u s . I n order t h a t the stroke arm have the samettravel as p r e v i o u s l y , the r a t i o of stroke arm t r a v e l t o cam f o l l o w e r t r a v e l had t o be i n c r e a s e d , r e s u l t i n g i n a more r a p i d stroke w i t h a more abrupt stop. Runs 26 t o 32 were made us i n g cam' A forward i n some runs and reversed i n o t h e r s , w i t h and without i n . and 5/16 i n . spacers. These r e s u l t s gave va r i o u s s i z e d regions of s i n g l e drops when p l o t s were, made i n which volume per stroke was p l o t t e d against strokes per second. However i t appeared t h a t the f l u c t u a t i n g temperature of the room where the experiments were being c a r r i e d out had more e f f e c t than the other v a r i a b l e s . The apparatus was then moved to'Constant Temperature Room"where f o r some of the time the temperature was s t i l l f a r from constant, v a r y i n g from 23°G t o 27°C. Nevertheless the r e s u l t s from Runs 26 - 32 d i d i n d i c a t e t h a t the abrupt f i n i s h t o the discharge stroke as obtained by cam A forward, and by the use o f spacer pieces on the cam f o l l o w e r d i d not increase the area of the " s i n g l e drop without t r a i l e r s " r e g i o n on the p l o t s of drop volume versus pump strokes per second. Figure 18 shows a p l o t of Run 35 where cam A was reversed, the temperature of the system maintained between 22.4° and 23 .0°C, and the n-butanol i n j e c t e d through a 5/32 i n . I.D. n o z z l e . L E G E N D 50 -2 40 UJ o cc h-111 30 -20 -3 O > I 0 O I DROP a 0 TRAILER 0 I DROP a I TRAILER + 2 DROPS a I TRAILER 0 3 DROPS a I TRAILER LIMIT OF APPARATUS 3 D R 0 p S & ^ T RML£« I DROP a I T R A I L E R ^ — f r ERRATIC - I DROP a I T R A I L E R / S T R O K E 1 .. 0 0 50 100 1-50 PUMP S T R O K E S / SEC. FIGURE 18 RUN 35 T Y P E S OF DROPS PRODUCED AND REGION OF SINGLE DROPS 5 / 3 2 " I.D. STAINLESS S T E E L N O Z Z L E C A M "A" R E V E R S E D n - B U T A N O L and W A T E R 2 0 0 ( i i i ) Examination of drops produced w i t h brass n o z z l e s . As considerable d i f f i c u l t y was experienced by the Department workshop i n manufacturing sharp edged s t a i n l e s s s t e e l nozzles as described by Greene ( 2 0 ) , brass n o z z l e s , being e a s i e r t o machine, were used f o r the remainder of t h i s i n v e s t i g a t i o n w i t h the exception of b r i e f study w i t h a T e f l o n n o z z l e . A comparison between the r e s u l t s of Run 35 ( f i g u r e 18} 5/32 i n . s t a i n l e s s s t e e l nozzle) and Run 39 ( f i g u r e 20, 5/32 i n . brass n o z z l e ) , a l l other c o n d i t i o n s being as n e a r l y "as p o s s i b l e the same, showed very l i t t l e d i f f e r e n c e r e s u l t i n g from the change, ( f i g u r e 5 4 ) . Table 7 l i s t s the runs made w i t h the sharp-edged brass nozzles i n t h i s study of the n-butanol-water system. Results from Runs 38-47 i n c l u s i v e ( f i g u r e s 19 - 28) showed t h a t drops without t r a i l e r s were produced i n the n-butanol-water system by the 5/32 i n . I.D. n o z z l e s , but none were produced by the 1/8 i n . and 3/16 i n . I.D. n o z z l e s . An a d d i t i o n a l n ozzle of 11/64 i n . I.D. was then made, being between the 5/32 i n . nozzle and the 3/16 i n . nozzle s i z e s . The " l i m i t of apparatus" shown i n f i g u r e s 18 t o 23 represents the upper l i m i t of r e l i a b i l i t y . Above t h i s volume per stroke of approximately 53 x 10"3 ml. the pump discharge was e r r a t i c . TABLE NO. 7 RUNS MADE WITH BRASS NOZZLES WITH N-BUTANOL-WATER SYSTEM. Run Nozzle s i z e Cam Spacer. Temperature F i g . Data Book* No. I . D. t h i c k n e s s . No. pages -inches inches °C • 38 5/32 A forward n i l 21 .7 -22 .6 19 7103, -6 39 5/32 A reversed n i l "21 .8 -23 .1 20 7104-5 40 5/32 • A forward I 22 .0 -22 .1 21 7107-8 41 5/32 B S.H.M. n i l 2 1 . 5 - 2 2 . 0 22 J109-10 42 5/32 A forward n i l (cam r e p a i r e d ) 22 .7 -23 .4 23 7111-2 43 1 /8 A forward n i l 2 2 . 6 - 2 2 . 9 24 7113-4 44 1/8 A reversed n i l 2 2 . 8 - 2 3 . 5 25 7115-6 44A 1 /8 B S.H.M. n i l 24 .0-24 .1 - 7117 45 3/16 B S.H.M. n i l 22 .5 -22 .6 26 7118 46 3/16 A forward n i l 2 2 . 7 - 2 2 . 9 27 7119 47 3/16 A reversed n i l 2 2 . 5 - 2 2 . 9 28 7120 51 11/64 A forward n i l 22.6-24 .0 29 7124-5 52 11/64 A reversed n i l 22 .8 -23 .4 30 7126-7 53 11/64 B S.H.M. (nozzle: con-taminated) n i l 2 2 . 6 - 2 2 . 9 31 7128 54 11/64 A forward n i l 22.8-24 .1 v 32 , 7133 55 11/64 B S.H.M. n i l 2 2 . 8 - 2 3 .a 33 •7133-4 * Log books, Dept. of Chemical Engineering, U n i v e r s i t y ~ of B r i t i s h Columbia L E G E N D 0 50 I 00 1-50 2 0 0 PUMP STROKES / SEC. FIGURE 19 RUN 3 8 T Y P E S OF DROPS PRODUCED AND REGION OF SINGLE DROPS 5 /32" I.D. BRASS NOZZLE CAM "A" FORWARD n . -BUTANOL and WATER _j i : i L_ 0 5 0 I 00 150 2 0 0 PUMP STROKES / SEC. FIGURE 20 RUN 39 TYPES OF DROPS PRODUCED AND REGION OF SINGLE DROPS 5 / 3 2 " I.D. BRASS NOZZLE CAM TTAA REVERSED n -BUTANOL and WATER L E G E N D O O I DROP & 0 TRAILER 1 DROP ft I TRAILER 2 DROPS ft I TRAILER MORE THAN I DROP LIMIT OF APPARATUS I DROP a TRAILER -9" ERRATIC - I DROP a 0 »| " I TRAILER 0 S T R O K E "I _L 0 50 00 PUMP 50 STROKES / SEC. FIGURE 21; RUN 40 T Y P E S OF DROPS PRODUCED AND REGION OF SINGLE DROPS 5 / 3 2 " I.D. B R A S S N O Z Z L E CAM "A" F O R W A R D , l/4 u S P A C E R n - B U T A N O L and W A T E R 2 00 L E 6 E N D O I DROP a 0 TRAILER 9 I DROP a I TRAILER LIMIT OF APPARATUS * 2 DROPS & I TRAILER E R R A T I C " I DROP a I TRAILER / S T R O K E 0 . •• " 0 » / i » 0-50 100 1-50 200 PUMP STROKES / SEC. FIGURE 22 RUN 41 T Y P E S O F DROPS PRODUCED AND REGION OF SINGLE DROPS 5 / 3 2 " I.D. BRASS N O Z Z L E CAM " B " n - B U T A N O L and W A T E R L E G E N D LIMIT OF APPARATUS 50 -O Q 4 or DROP a DROP a 2 DROPS a 3 DROPS a ro 40 J o 30 MORE THAN 3BR0PS &ITRAILER -«f #-TRAILER TRAILER TRAILER TRAILER I DROP tr C O 20 L L ) O > TRAILER I 0 - " 0 ERRATIC- I DROP a I TRAILER / STROKE 0 / 0 0-50 100 150 PUMP STROKES / SEC. FIGURE 23 R U N 4 2 T Y P E S OF DROPS PRODUCED AND REGION O F SINGLE DROPS 5 / 3 2 " I.D. BRASS N O Z Z L E CAM "A" FORWARD (REPAIRED) n - B U T A N O L and W A T E R 200 LEGEND Q I DROP & I TRAILER 6 I DROP a 2 TRAILERS ro E R R A T I C - I DROP a I T R A I L E R / S T R O K E 0 it ii 0 II / II — J 1 I L_ 0-50 1 0 0 1-50 2 0 0 P U M P S T R O K E S / S E C . FIGURE 24 RUN 4 3 TYPES OF DROPS PRODUCED 1/8 " I.D. BRASS NOZZLE CAM "A" FORWARD n-BUTANOL and WATER LEGEND t DROP a I TRAILER I DROP a 2 TRAILERS 1 DROP a 3 T R A I L E R S O BO UNCE 2 DROPS a TRAILERS 3 DROPS a T R A I L E R S -o 2 TRAILERS/DROP -6 ®-2 DROPS a TRAILERS DBOP MORE THAN I DROP - O — ^ T R A I L E R S / DROP a TRAILER ERRATIC - I DROP a I TRAILER / S T R O K E 0 M " 0 » / II ! t 0-50 00 1-50 PUMP STROKES / SEC FIGURE 25 RUN 4 4 TYPES OF DROPS PRODUCED 1/8" I.D. BRASS NOZZLE CAM "A" REVERSED n- BUTANOL and WATER 2 00 rO 4 0 30 L E G E N D Q I DROP a I T R A I L E R 6 I DROP a 2 TRAI L E R S -O I DROP a 3 TRAI L E R S O- B O U N C E . LU o cr »-co \ UJ 2 _J O > 20 0 - O TRAILER / DROP 2 Q_ -O— 3 TRAILERS / DROP JL • " 9 A 2 TRAILERS . / DROPc) O 6 o——5—O——— o-ERRATIC — I DROP a I T R A I L E R / S T R O K E " 0 JL 0 0 50 i 00 I 50 PUMP STROKES / S E C . 2 00 FIGURE 26 RUN 4 5 T Y P E S O F DROPS P R O D U C E D 3/16" I.D. B R A S S N O Z Z L E CAM " B " n - BUTANdL and WATER GE ND a I T R A I L E R a 2 TRAILERS a 3 TRAILERS a 4 TRAILERS E R R A T I C - I DROP a I T R A I L E R / S T R O K E 0 « » 0 » / " 0 0-50 100 150 PUMP S T R O K E S / SEC FIGURE 27 TYPES OF DROPS PRODUCED 3/16" I.D. BRASS NOZZLE CAM 'K FORWARD n-BUTANOL and WATER RUN 46 L E G E N D Q I DROP a I TRAILER 6 I DROP a 2 T R A I L E R S -O I DROP a 3 T R A I L E R S ' O- B O U N C E 4 0 -m 6 X ERRATIC I DROP a I T R A I L E R / STROKE \ I I I L_ 0 0 5 0 100 I 50 2 00 PUMP STROKES / SEC FIGURE 28 RUN 47 T Y P E S O F DROPS PRODUCED 3/16" I.D. B R A S S N O Z Z L E CAM "A" R E V E R S E D n - B U T A N O L and W A T E R M U L T I P L E DROPS a TRAILERS LIMIT I \ OF \ APPARATUS DROPS WITH MULTIPLE TRAILERS REGION OF SINGLE DROPS - ZERO TRAILERS OL 1 1 1 0-50 •00 •50 2 00 2-50 300 PUMP STROKES / SEC. 3-50 4-00 F I G U R E 29 REGION OF SINGLE DROPS 11/64" I.D. BRASS NOZZLE CAM "A" FORWARD n-BUTANOL and WATER RUN 51 LIMIT OF'APPARATUS OJ I I I I I I I ! ! I I I I L 0-50 1-00 150 200 2-50 300 3 50 4 00 4-50 500 5-50 6 00 6-50 7-00 PUMP STROKES / SEC. FIGURE 30 REGIONS O F SINGLE DROPS 1 1 / 6 4 " I.D. B R A S S N O Z Z L E C A M " A 1 * R E V E R S E D n - B U T A N O L and W A T E R R U N 5 2 50 LIMIT OF APPARATUS 40 ro O x 30 LU o cc 20-1-UJ 3 O > 0 REGION O F SINGLE D R O P S - Z E R O T R A I L E R S 0'50 100 •50 2 00 2-50 PUMP STROKES/S E C . FIGURE 31 REGION OF SINGLE DROPS 11/64" I.D. BRASS NOZZLE CAM "B" n-BUTANOL.and WATER RUN 53 3 0 0 3-50 4 0 0 4-50 LIMIT OF APPARATUS 50f-ro 404-i o 30| UJ O rr f-co 201 UJ S 3 5 .01 NO SINGLE DROPS L O C A T E D BEYOND I 0-50 •00 1-50 PUMP S T R O K E S / S E C . FIGURE 32 2 0 0 2-50 3 0 0 REGION OF SINGLE DROPS 11/64" I.D. BRASS NOZZLE C A M A FORWARD n - BUTANOL and WATER RUN 54 REPETITION OF RUN 51 LIMIT OF APPARATUS PUMP STROKES / SEC. FIGURE 33 RUN 55 11/64" I.D. BRASS NOZZLE REGIONS OF SINGLE DROPS CAM 11 B " n-BUTANOL and WATER REPETITION OF RUN 53 72 Runs 51 , 52 and 53 were made w i t h the 11/64 i n . I.D. nozzle ( f i g u r e s 29,30 and 31) and much l a r g e r regions of s i n g l e drops without t r a i l e r s found than w i t h the 5/32 i n . I.D. n o z z l e . However at the end of Run 5 2 , w i t h s t r o k e s per second at 7.75 and volume of drop at 8 . 6 0 x 10" ^  rai. the nozzle t i p became wetted on one si d e by the n-butanol. A s i m i l a r occurrence was observed i n Run 53 at 4 .13 strokes per second and 21 .2 x 10~3 ml. Figure 34 (photographs 5 5 - 2 0 Run 53 , Frames 2CD and 21) shows the drop formation before and a f t e r the t i p was wetted w i t h the n-butanol under these c o n d i t i o n s . A new 11/64 i n . I.D. sharp-edged nozzle was made, but t h i s , , being of s l i g h t l y l a r g e r diameter (Appendix A), gave d i f f e r e n t r e s u l t s from those obtained by the former 11/64 i n . n o z z l e , before w e t t i n g . This nozzle however became wetted by the nebdtanol i n a very few minutes. The 5/32 i n . n o z z l e used i n the e a r l i e r Runs 38-42 was f i t t e d i n the apparatus, and a f t e r a few minutes of op e r a t i o n was wetted at the t i p , although i n Runs 38-42 such wetting d i d not occur as confirmed by s t i l l and movie photographs ( f i g u r e 4 9 a ) . No s i n g l e drops without t r a i l e r s were produced while the t i p was wetted by the n-butanol. Run 53 Frame 20 Before contamination Run 53 Frame 21 A f t e r contamination FIGURE 34 E f f e c t s of Contamination 11/64 i n . I.D. brass n o z z l e , Cam " B " . n-butanol and water system 74 This evidence pointed s t r o n g l y t o i n t e r n a l con-tam i n a t i o n a f f e c t i n g the surface t e n s i o n s of e i t h e r or both of the n-butanol and the water. Suspicions were aroused over the p o s s i b i l i t y of contamination i n the Winchester of d i s t i l l e d water being used. The b o t t l e used up t o the end of Run 49 now contained methyl i s o b u t y l ketone being s a t u r a t e d w i t h d i s t i l l e d water, f o r the f u t u r e i n v e s t i g a t i o n of the methyl i s o b u t y l ketone - water system. I n i t s place a new "cle a n " b o t t l e was r i n s e d out, f i r s t w i t h tap water, and l a t e r w i t h d i s t i l l e d water, before being f i l l e d w i t h d i s t i l l e d water. D i s t i l l e d water was then s t o r e d i n t h i s b o t t l e i n the Constant Temperature Room so as t o be at the temperature of the apparatus when added t o I t . Surface t e n s i o n measurements were made w i t h a #70540 type Cenco-du Nouy P r e c i s i o n I n t e r f a c i a l Tensiometer u s i n g a #70542 type Platinumaand I r i d i u m Ring, on the n - l u t a n o l i n the apparatus, the unused n-butanol, the d i s t i l l e d water, and on the d i s t i l l e d water from the suspected storage b o t t l e , as shown i n t a b l e 8. From these readings both the b o t t l e water and the n-butanol t h a t wet the nozzle had dropped i n surface t e n s i o n . These f i n d i n g s pointed t o the entrance of a t r a c e of "Calgon" i n t o the system from the storage b o t t l e . T h i s c l e a n s i n g agent i s used f o r c l e a n i n g out the glassware i n the TABLE NO. 8 SURFACE TENSION MEASUREMENTS TO DETERMINE PRESENCE OF CONTAMINATION M a t e r i a l s Surface t e n s i o n Maximum Temp, Dynes/cm d e v i a t i o n from the mean of 4 - 6 readings taken Dynes/cm Pure d i s t i l l e d water 77.1 Water from b o t t l e 64 .7 Unused n-butanol 27.5 Unused n-butanol saturated with,pure d i s t i l l e d water 27.8 Former saturated n-butanol from apparatus before c ont aminat i o n 27.7 Saturated n-butanol from contaminated apparatus 26.9 0.3 0.0 0.0 0.1 0.1 0.0 69°F Department s t o r e s , and probably there was a t r a c e of the agent l e f t I n the b o t t l e , even though the b o t t l e had been r i n s e d w i t h d i s t i l l e d water p r i o r t o being f i l l e d w i t h i t . Both the water and the n-butanol were re p l a c e d i n the apparatus and the nozzles cleaned i n acetone. The nozzles were s t i l l wetted at the t i p s by the n-butanol. B o i l i n g the nozzles i n d i s t i l l e d water helped, but s t i l l t here was a tendency f o r the n-butanol t o wet the t i p . F i n a l l y , by a c c i d e n t , i t was found t h a t by heating the nozzle u n t i l the brass j u s t changed c o l o u r and then plunging i t i n t o d i s t i l l e d water, t h a t the water wet the n o z z l e . "Flamed" nozzles t r e a t e d i n t h i s way, then worked s a t i s f a c t o r i l y , and , i n p a r t i c u l a r , the 5/32 i n . and 11/64 i n . I.D. nozzles were no longer wetted by the n-butanol. Runs 54 and 55 ( f i g u r e s 32 and 33) reproduce reasonably w e l l the r e s u l t s of Runs 51 and 53 r e s p e c t i v e l y ( f i g u r e s 29 and 31) made before the contamination. ( i v ) Examination of drops produced w i t h a T e f l o n -. t i p p e d n o z z l e . T e f l o n was chosen f o r examination as i t i s h i g h l y hydrophobic and would be wetted p r e f e r e n t i a l l y by n-butanol r a t h e r than by water. A c c o r d i n g l y an 11/64 i n . I.D. T e f l o n t i p p e d nozzle^ was used f o r Run 48 w i t h cam A forward, and f o r Run 49 w i t h Gam A reversed. Figures 35 and 36 show the r e s u l t s of these examinations and f i g u r e 37 shows the n-butanol w e t t i n g the t i p of the n o z z l e . No s i n g l e drops without t r a i l e r s were found. This examination w i t h the T e f l o n nozzle concluded the experimental work w i t h the n-butanol and water system. The apparatus, was then prepared f o r the experimentation w i t h the second system, methyl i s o b u t y l ketone and water as described i n the next s e c t i o n . LEGEND ro40 6 9 I DROP a I TRAILER 6 I DROP a 2 TRAILERS - O I DROP a 3 TRAILERS O BOUNCE £30»-LU O CC LU 3' > — 6 o-2 TRAILERS /DROP , ^ 2 TRAILERS /. DROP 6— - o -TRAILER / DROP o BOUNCE O — I TRAILER / DROP -9-r^-ERRATIC - I DROP 8 I . T R A I L E R / S T R O K E 0 " "0 " / " I I -9-0-50 00 1-50 PUMP S T R O K E S / SEC F I G U R E . 35 TYPES OF DROPS PRODUCED 11/64" I. D. TEFLON NOZZLE CAM '8' FORWARD n-BUTANOL and WATER 2 00 LEGEND 4 C -ro i O 3 C-LU O cr r-V) 2 C -LU —I I Cf-o > 0 o . 9-- o -9- -9-ERRATIC Q I DROP a .1 TRAILER 6 I DROP a 2 TRAILERS -O I DROP a 3 TRAILERS O BOUNCE 2 TRAILERS / DROP -6 - 6 -6-I TRAILER / DROP — B O U N C E O I TRAILER / DROP — 9 -Q I DROP a I TRAILER. / STROKE 0 . . . . 0 " / " i ; i -Q-0 50 100 |-50 PUMP STROKES / SEC FIGURE 36 TYPES OF DROPS PRODUCED 11 /64" I.D. TEFLON NOZZLE C A M 'K REVERSED n - BUTANOL and WATER RUN 49 2 00 80 FIGURE 37 11/64 i n . I.D. T e f l o n Tipped Nozzle n-butanol and water system (D) EXPERIMENTAL WORK WITH THE METHYL ISOBUTYL KETONE AND . . . WATER SYSTEM The n-butanol was removed from the apparatus i n the f o l l o w i n g manner so as t o prevent a i r l e a k i n g i n t o the pump.system. The valve G ( f i g u r e 12) at the bottom of the a i r t r a p E was c l o s e d , the a i r vent valve F opened, and the plu g at the center top of the a i r t r a p removed. Through t h i s opening the n-butanol was removed by s u c t i o n from an a s p i r a t o r . To c l e a n out the n-butanol, f i r s t d i s t i l l e d water was f l u s h e d through by f i l l i n g the storage b o t t l e A l e a v i n g valve C open, and removing the water from the a i r t r a p . Second, the methyl i s o b u t y l ketone was f l u s h e d through as above, u n t i l i t was reasonably sure t h a t the water had been d i s p l a c e d . Then the a s p i r a t o r l i n e was removed, the plug re p l a c e d i n the a i r t r a p , vent valve F c l o s e d , and the storage b o t t l e A f i l l e d w i t h water s a t u r a t e d methyl i s o b u t y l ketone. The valve G at the bottom of the a i r t r a p was opened and the pump s t a r t e d immediately. The pump was run at high d e l i v e r y and moderate speed u n t i l the n-butanol i n i t had been d i s p l a c e d w i t h the methyl i s o b u t y l ketone. Each of the nozzles was cleaned by being r e -peatedly heated t o approximately 250°C. i n a Bunsen flame, and then plunged i n t o d i s t i l l e d water u n t i l the nozzle was wetted by the water. 82 The 1/8 i n . brass nozzle was then i n s t a l l e d i n the column and the column f i l l e d w i t h d i s t i l l e d water saturated w i t h methyl i s o b u t y l ketone. I t was observed t h a t the bellows valve pump l i m i t e d t o approximately 53 x 10" 3 ml. per stroke was inadequate i n c a p a c i t y f o r t h i s system which produced l a r g e r drops. Figure 38 shows an exploded view photograph of a l a r g e r bellows .pump. This was made from a §ln. x 3/4:in. bellows B soldered t o an adapter piece A w i t h an 1/8 i n . I . P i S . threaded hole through the centre l e a d i n g t o the i n s i d e of the bellows, and an e x t e r n a l thread t o mate w i t h the i n -t e r n a l thread of the body piece C. The body piece C f i t t e d over the o r i g i n a l bellows pump va l v e h o l d e r E and was h e l d i n p o s i t i o n by two set screws. I n s i d e the valve holder was a brass spacer piece D t o connect the rod cap F t o the end of the bellows B. Figure 38 shows a l s o the assembled pump. The check valves were those used w i t h the o r i g i n a l bellows valve pump. The new pump was capable of d e l i v e r i n g 120 x 10"" 3 ml. per stroke without s t r a i n i n g the cam operated a d j u s t a b l e stroke mechanism, and was i n a l l ways most s a t i s f a c t o r y . A cork stopper f i t t e d at the top of the round part of the columns i n l i e u of the neoprene stopper used w i t h the n-butanol and water system leaked i n s p i t e of a l l attempts t o make i t t i g h t . I n view of t h i s f a c t , a 83 polythene stopper was machined and d r i l l e d t o take the thermometer, f u n n e l and g l a s s tube. The leakage t h a t s t i l l took place at the thermometer, tube and f u n n e l connections was sealed by f i t t i n g a t i g h t hose clamp around the outside of the polythene stopper. The o p e r a t i o n of the e l e c t r i c counter was syn-chronized w i t h t h a t of the e l e c t r i c t i m er by p l a c i n g a s w i t c h i n s e r i e s w i t h the two d e v i c e s . The procedure f o r t a k i n g readings described on page 49 was a l t e r e d a c c o r d i n g l y . The s w i t c h was c l o s e d u n t i l the counter reached a con-venient number - u s u a l l y an even hundred, and then opened. The c l o c k was turned back t o zero. Valve C ( f i g u r e 12) was c l o s e d so. t h a t the pump supply came only from the b u r e t t e . Immediately the meniscus i n the b u r e t t e passed the zero mark the s w i t c h was c l o s e d , and not opened t i l l a g iven m i l l i l i t r e mark was reached. Thus the d i f f e r e n c e i n r e v o l u t i o n s , the time i n seconds, and the volume pumped were recorded ac-c u r a t e l y , e s p e c i a l l y at h i g h speeds. Eleven runs were made w i t h mutually saturated methyl i s o b u t y l ketone and water. Both the nozzle s i z e and the cam p r o f i l e were v a r i e d . Table 9 summarizes the experimental work c a r r i e d out w i t h t h i s system. 84 FIGURE 38 Bellows Pump TABLE NO. 9 D. EXPERIMENTAL INVESTIGATION METHYL ISOBUTYL KETONE-WATER SYSTEM Run Nozzle S i z e Cam Temperature P i g . Data Book •D. i n . inches F No. I. .No. . Page , o 56&56A 1/8 A forward 74.5-75.0 7136-7 57 1/8 A reversed 74.0-74.5 39 7138 58 1/8 A forward 73.0-75.5 40 7139 59 1/8 B S.H.M. 75.0-76.0 41 7140 60 11/64 B S.H.M. 72.O-73.O 42 7141 63 11/64 B S.H.M. 72.5 4 3 7143 64 11/64 A forward 72.5 44 7144-5 65 11/64 A reversed 73.0 7146 66 3/16 A forward 73.0 7146 6 7 7/64 A forward 72.5 45 7147 68 5/32 A forward 73.0 4 6 7148 LIMIT OF APPARATUS PUMP S T R O K E S / S E C . FIGURE 3 9 REGION OF SINGLE DROPS 1 / 8 " I.D. BRASS NOZZLE CAM "A" REVERSED METHYL ISOBUTYL KETONE and WATER RUN 57 iooh-ui I V J : — _ 1 1 ' 6-50 . I 00 I -50 2 00 PUMP STROKES / SEC. / ' FIGURE 40 REGION OF SINGLE DROPS 1/8" BRASS NOZZLE CAM "A" FORWARD METHYL ISOBUTYL KETONE and WATER RUN 58 >'*7 LIMIT OF APPARATUS 90 10 0 8 O 701 o DC 6 0 h ui => O > 50 - o REGION OF SINGLE DROPS - ZERO TRAILERS 4 0 I 1 0-50 100 1-50 P U M P S T R O K E S / S E C , FIGURE 41 REGION OF SINGLE DROPS 1/8" I.D. BRASS NOZZLE CAM "Bu METHYL ISOBUTYL KETONE and WATER RUN 59 200 2-50 S8 PUMP STROKES / SEC. FIGURE 42 REGION OF SINGLE DROPS 11/64" I.D. BRASS NOZZLE CAM "Bw CONTAMINATED METHYL ISOBUTYL KETONE and WATER RUN 60 » 90 1(20 0 LIMIT OF APPARATUS 0 9 0 rO O x 6 80 LU X 701 o OC *-t o Ui S 6 0 j o > 50 40 -0--O-— 0-50 •00 1-50 2-00 2-50 300 3-50 PUMP STROKES / SEC 400 4-50 500 5 50 6-00 6-50 700 FIGURE 4 3 REGION OF SINGLE DROPS II /64 n BRASS NOZZLE CAM M B 9 METHYL ISOBUTYL KETONE and WATER RUN 6 3 20 LIMIT OF APPARATUS I t 0 I—" IOO \r 90 ro O x> E 80 LU o 70 OT LU 3 o 60 > 50 REGION OF SINGLE DROPS - ZERO TRAILERS 40 X 0 50 100 . 1-50 200 2-50 3 00 3-50 PUMP STROKES / SEC FIGURE 44 REGION OF SINGLE DROPS 11/64-** I.D. BRASS NOZZLE CAM "A" FORWARD METHYL ISOBUTYL KETONE and WATER RUN 64 4 0 0 450 5 00 5-00 6 0 0 LIMIT OF A P P A R A T U S NO REGIONS FOUND BEYOND IOO P U M P S T R O K E S FIGURE 45 REGION OF SINGLE DROPS 7/64" I.D. BRASS NOZZLE CAM "A" FORWARD METHYL ISOBUTYL KETONE ond WATER RUN 67 P U M P STROKES / SEC FIGURE 46 * REGION50F SINGLE DROPS 5/32" I. D. BRASS NOZZLE CAM "A" FORWARD . METHYL ISOBUTYL KETONE and WATER RUN 68 During the runs 56 and 56A the methyl i s o b u t y l ketore-water system g r a d u a l l y became contaminated. Probably t h i s contamination i*as due t o the l e a c h i n g out of the p l a s t i c i z e r i n the polythene of the stopper at the top of the column, or t o the d i s s o l v i n g of s m a l l neoprene "0" r i n g between the nozzle and the adapter. As e i t h e r or both of the above reasons may have been r e s p o n s i b l e , the ap-paratus was f l u s h e d out a f t e r Run 56, t h i s run being repeated l a t e r as Run 5 8 . As each of Runs 60, 61 and 62 could not be reproduced the apparatus was allowed t o stand f o r a week to give the methyl i s o b u t y l ketone time t o d i s s o l v e t t h e contaminants. Then the methyl i s o b u t y l ketone and water was replaced w i t h mutually saturated methyl i s o b u t y l ketone and water, the nozzle flamed and the neoprene "0" r i n g replaced w i t h " T e f l o n " . A f t e r these treatments there appeared to be no f u r t h e r contamination. I n view of the regions of s i n g l e drops w i t h the 1/8 i n . I.D. nozzle ( f i g u r e s 39,40 and 41),a 7/64 i n . I.D. nozzle was made and s t u d i e d ( f i g u r e 4 5 ) . The range of s i n g l e drops w i t h t h i s l a t t e r nozzle was s m a l l . The 11/64 i n . I.D. nozzle produced a l a r g e r e g i o n of s i n g l e drops ( f i g u r e s 42, 43 and 4 4 ) , and the 5/32 i n . I.D. nozzle ( f i g u r e 46) produced a much sma l l e r r e g i o n . The- 3/16 i n . I.D. nozzle f a i l e d to produce single drops -per.stroke. The methyl i s o b u t y l ketone flowed out i n unstable spurts consisting of a;;-.series of drops . of varying size from down inside -the nozzle. With a small range of single drops without t r a i l e r s from the 7/64 i n . I.D. nozzle and no single drops from the 3/l6 i n . I.D. nozzle, the range of nozzle sizes was con-sidered to be adequately investigated. 96 RESULTS AND DISCUSSION '• The p r e l i m i n a r y examination u s i n g the d i e s e l i n j e c t i o n pump f o r pumping the dispersed phase n-butanol i n t o the continuous water phase provided data on drop shape and s i z e . The photographic arrangement r e c o r d i n g two. views of the. drops at r i g h t angles simultaneously, gave a f i e l d of view of n e a r l y 2 inches v e r t i c a l height at the n o z z l e . As the d i s t o r t i o n o s c i l l a t i o n caused by the formation of the drop was damped out i n t h i s d i s t a n c e , these photographs showed the " t r u e " drop shape. By p r o j e c t i n g these photo-graphs by means of a s t r i p f i l m p r o j e c t o r on a la r g e sheet of graph paper, the drop axes could be measured e a s i l y . The p o s i t i o n of the graph paper was arranged so t h a t the 1/8 i n . nozzle t i p i n Runs 6 - 1 1 covered 25 s m a l l squares i n width, and t h e r e f o r e each s m a l l square represented 0.005 i n . S i m i l a r l y , when measuring the drops i n Runs 12 and 13 the 5/32 i n . nozzle t i p covered 31.25 squares. Table 10 shows the r e s u l t s of these measurements f o r Runs 12 and 13 i n which the 5/32 i n . I.D. nozzle was used. "X" and "y" represent the two p e r p e n d i c u l a r h o r i z o n t a l axes, and " z " the v e r t i c a l ( f i g u r e l ) . Examination of the r e s u l t s i n Table 10 shows that except i n one case (run 13, frame 2) the values of "x" and "y" vary no more than those of " z " , i n d i c a t i n g t h a t the h o r i z o n t a l axes are both equal and the h o r i z o n t a l s e c t i o n a c i r c l e . The d e v i a t i o n i n Run 13, frame 2, could have been TABLE NO. 10 Measurement of drop s i z e s by p r o j e c t i o n on graph paper u s i n g a s l i d e - s t r i p f i l m projector... Run Frame Dimensions of Drop Axes. No. .of No. ... i n . x 0.005 T r a i l e r s , 12 13 Dia. of s p h e r i c a l T r a i l e r s , i n . x 0.005 L e f t .. x view Right z z view y 2 .. . 23 .13 .13 . 23 0 .7 32 12 13 32 9 . . 3 0 14 13 . . 30 3 5 , 5 , 14 17 12 I l l 17 2 3 , .3 16 19 12 12 19 0 18, 15 11 11 i 4 | 1 1 0 | ** 2 . . 16 11 10 23 0 * 6 2 0 io|. 20 0 . 7 . .27 - 1 0 | ..27 1 8 19: .11 11. 19. 0 .9. 17 i o | iQi 171 0 10. ... 19 1 0 | 11 1 8 | 0 11 . 18. 11 12 19 5 4, 3 , x and y an£ h o r i z o n t a l axes of drops z i s v e r t i c a l a x i s of drops' 98 due t o t i l t of the drop. These r e s u l t s i n d i c a t e the drop shape t o he oblate spher&fcl&lwithin the s i z e range covered by the t a b l e . The r e s u l t s of Greene (20) could not be r e -produced i n t h i s i n v e s t i g a t i o n although the d e t a i l e d study made i n Runs 1-11 i n c l u s i v e was made usi n g the same pump, nozzle and system. Runs 26-32 showed th a t the e f f e c t of the temp-erature was s i g n i f i c a n t i n the production of uniform drops. This v a r i a b l e was p a r t i a l l y e l i m i n a t e d by conducting the remainder of the i n v e s t i g a t i o n i n the "Constant Temperature Room". The main i n v e s t i g a t i o n showed t h a t nozzle i n s i d e diameter s i z e was very c r i t i c a l f o r the formation of s i n g l e drops w i t h systems of very low i n t e r f a c i a l t e n s i o n . With n-butanol-water system, the 5/32 i n . I.D., and 11/64 i n . I.D. nozzles produced regions of uniform drops ( f i g u r e s 47, 48, 49 and 50), while 1/8 i n . I.D. and 3/l6 i n . I.D. d i d not ( f i g u r e s 49 and 50). The former nozzle t i p s were p r e f e r - ^  e n t i a l l y wetted by the water and the l a t t e r by the n-butanol. The range of nozzle s i z e t h a t produced s i n g l e drops 1 w i t h the methyl i s o b u t y l system was from 7/64 i n . I.D. t o 11/64 i n . I.D. ( f i g u r e s 51 and 52). This range was consider-a b l y g r e a t e r than w i t h the system of n-butanol-water of lower 9 9 Run 3 6 Frame 3 FIGURE 47 S i n g l e Drops without T r a i l e r s 5 / 3 2 i n . I.D. s t a i n l e s s s t e e l nozzle 1/4 i n . spacer and Cam "A" reversed 2 9 . 0 x 10" 3 m i . per stroke 1.00 strokes per second n-butanol and water system Run 37 Frame 15 FIGURE 48a S i n g l e Drops without T r a i l e r s 5/32 i n . I.D. s t a i n l e s s s t e e l n o z z l e , Cam "A" forward 38.5 x 10"3 ml. per stroke 1.00 strokes per second n-butanol and water system Run 37 Frame 16 FIGURE 48b S i n g l e Drops without T r a i l e r s 5/32 i n . I.D. s t a i n l e s s s t e e l n o z z l e , Cam "A" forward 5 0 . 0 x 10" 3 ml. per stroke 1.16 strokes per second n-butanol and water system Run 42 Frame 2 FIGURE 49a 28.6 X 10 S i n g l e Drops without T r a i l e r s 5/32 i n . I.D. brass n o z z l e , Cam v i r r 3 m n-butanol and water system " A " forward l. per strokes O.692 strokes per second Run 43 Frame 15 FIGURE 49b One Drop and One T r a i l e r 1/8 i n . I.D. brass n o z z l e , Cam " A " forward 32.3 x 10~3 ml. per strokes 1.295 strokes per second n-butanol and water system 102 Run 46 Frame 9 FIGURE 50a One Drop and Two T r a i l e r s 3 / l 6 i n . I.D. brass n o z z l e , Cam "A" forward 21.3 x 10" 3 ml. per stroke 1.16 strokes per second n-butanol and water system Run 51 Frame 22 FIGURE 50b S i n g l e Drop without T r a i l e r 11/64 i n . I.D. brass n o z z l e , Cam "A" forward 35»8 x 10~3 ml. per stroke 3.45 strokes per second n-butanol and water system 103 Run 56 Frame 4 FIGURE 51a S i n g l e Drops without T r a i l e r s 1/8 i n . I.D. brass n o z z l e , Cam "A" forward 8 3 . 3 x 10~3 ml. per stroke 0.254 strokes per second Methyl I s o b u t y l ketone and water Run 56 Frame 13 FIGURE 51b S i n g l e Drops without T r a i l e r s 1/8 i n . I.D. brass n o z z l e , Cam "A" forward 6 6 . 7 x 10 - - 5 ml. per stroke 1.18 strokes per second Methyl i s o b u t y l ketone and water 104 Run 67 Frame 4 FIGURE 52a S i n g l e Drops without T r a i l e r s 7/64 i n . I.D. brass n o z z l e , Cam "A" forward 31.7 x 10~3 ml. per stroke 1.43 strokes per second Methyl I s o b u t y l ketone and water Run 68 Frame 6 FIGURE 52b S i n g l e Drops without T r a i l e r s 5/32 i n . I.D. brass n o z z l e , Cam "A" forward 129.0 x 10" 3 ml. per stroke 1.74 strokes per second Methyl i s o b u t y l ketone and water 195 interfacial tension. The region of single drops produced with the 7/64 i n . I.D. nozzle was small, 1/3 i n . I.D. and 5/32 i n . I.D. larger, and that with the 11/64 in. I.D. nozzle large. The 3/l6 in. I.D. nozzle produced non uniform drops i n spurts of several drops at a time. Appendix A gives the inside diameter of the nozzles measured accurately with a travelling microscope. The preferential wetting of the nozzle t i p by the continuous phase rather than by the dispersed phase appeared to be most important for the formation of single drops. At no time were single uniform drops without t r a i l e r s observed when the t i p of the nozzle was wetted by the dispersed phase. Two general patterns were observed when plots were made of volume per stroke against pump strokes per second. The f i r s t pattern was obtained when the dispersed phase wetted the nozzle t i p , and the second when the continuous phase wetted the nozzle t i p . When the dispersed phase wetted the nozzle t i p , small t r a i l e r s followed the larger drops, and "bounce" (where the small t r a i l e r drop accelerated, collided with the main drop and bounced off to one side) was present. The volume per stroke for bounce, and also the minimum volume for a drop to be formed at each stroke, each appeared to be i o 5 independent of pump strokes per second, and of the cam p r o f i l e used. Regardless of nozzle s i z e , n ozzle m a t e r i a l , or cam p r o f i l e , so long as the dispersed phase wetted the nozzle t i p , the same general p a t t e r n r e s u l t e d and no s i n g l e drops without t r a i l e r s were formed, ( f i g u r e s 17 and 24 t o 28). However, when the continuous phase wetted the nozzle t i p , f o r a given temperature, system and n o z z l e , the r e s u l t i n g patterns showed a c h a r a c t e r i s t i c shape. These patterns d i d vary t o some degree w i t h cam p r o f i l e as shown i n f i g u r e s 19 t o 23 "and a l s o when spacers were used t o l i m i t the t r a v e l of the cam f o l l o w e r ( f i g u r e 8) as shown i n f i g u r e 53 where the p l o t of Run 40 i s superimposed on the p l o t of Run 42. The drops formed outside the regions of s i n g l e drops i n the p l o t s where the continuous phase wetted the nozzle t i p c o n s i s t e d of one s m a l l t r a i l e r and one or more l a r g e r drops of approximately the same s i z e . The e f f e c t of changing nozzle m a t e r i a l from s t a i n l e s s s t e e l t o brass was s m a l l . F i g u r e 54 shows the p l o t of Run 35 superimposed on t h a t of Run 39 . Hun 35 was made w i t h a 5/32 i n . I.D. nozzle made w i t h s t a i n l e s s s t e e l and Run 39 w i t h b r a s s , a l l other c o n d i t i o n s being the same. However, the change from 11/64 i n . I.D. brass nozzle t o a 11/64 i n . I.D. " T e f l o n " nozzle (the l a t t e r being s t r o n g l y hydrophobic) caused the nozzle t i p t o be wetted by the n-butanol, and then the p l o t s took the general p a t t e m f o r nozzles wetted by the dispersed phase. ERRATIC-1 DROP a I TRAILER / STROKE . , 0 " " 0 " | / " | | 0 0-50 100 1-50 2 00 PUMP S T R O K E S / SEC FIGURE §3 E F F E C T OF CAM SPACER FIGURES 2*8 23 SUPERIMPOSED n-BUTANOL and WATER ERRATIC — I DROP" ft I T R A I L E R / S T R O K E • | 0 " " 0 | " / " | , 0 0-50 1 0 0 1-50 2 0 0 PUMP S T R O K E S / S E C F I G U R E 5 4 S T A I N L E S S S T E E L ft B R A S S N O Z Z L E S F I G U R E S 18 8 20 SUPERIMPOSED n - B U T A N O L on3 WATER A l s o observed In t h i s i n v e s t i g a t i o n was the very-l a r g e e f f e c t of surface a c t i v e agents on drop formation. The very small t r a c e amount of contaminant t h a t must have been present i n Runs 52 and 53 caused the nozzle t i p s t o become wetted by the n-butanol. Figure 34 shows photographs of the drop formation j u s t before and j u s t a f t e r the w e t t i n g of the nozzle t i p by the n-butanol had taken p l a c e . Even a f t e r the system was f l u s h e d out, the nozzle t i p was wetted s t i l l by the n-butanol. Only by h e a t i n g the nozzle t o d i s c o l o u r a t i o n temperature and then plunging i t i n t o d i s t i l l e d water was the nozzle t i p once again p r e f e r e n t i a l l y wetted by the .water. From examination of the l i t e r a t u r e i t was found that Buchanan (15) had discovered t h a t when brass and aluminum o r i f i c e p l a t e s were heated t o about 600°C and quenched i n kerosene, both e x h i b i t e d wetted drop formation when kerosene was d i s p e r s e d through them. However when they were quenched i n water, they e x h i b i t e d non-wetted drop formation w i t h kerosene. ("Wetted drop formation" was the production of drops at a p l a t e wetted by the dispersed phase). Figure 42 shows the r e g i o n of s i n g l e drops obtained i n Run 60 w i t h the 11/64 i n . I.D. brass nozzle and the methyl i s o b u t y l ketone system contaminated. Figure 43 shows the r e g i o n of s i n g l e drops obtained i n Run 63 a f t e r the contents of the apparatus had been re p l a c e d and the nozzle "flamed". 2M The r e p r o d u c i b i l i t y of the r e s u l t s where the nozzle t i p was wetted by the n-butanol i n Runs 14 t o 24 i n c l u s i v e i s shown i n f i g u r e 17. Since the experimental work was c a r r i e d out over a p e r i o d of time from May 16th t o 29 th , 1962, the f a c t that the s c a t t e r of r e s u l t s i s reasonably s m a l l i n d i c a t e s t h a t the r e p r o d u c i b i l i t y was good. However, the r e p r o d u c i b i l i t y of the r e s u l t s where the nozzle t i p was not wetted by the n-butanol was not so good. This f a c t was undoubtedly due t o the c r i t i c a l nature of the wetting preferences of the phases on the nozzle t i p . Run 54 , f i g u r e 32 was a r e p e t i t i o n of Run 5 1 , f i g u r e 29 , but had no r e g i o n of s i n g l e drops at h i g h strokes per second as had Run 51« The nozzle i n Run 54 had been "flamed" a f t e r the contamination i n Run 53* and i t s surface c o n d i t i o n may have been changed s l i g h t l y . Run 55 ( f i g u r e 33) was a r e p e t i t i o n of Run 53 , ( f i g u r e 3.1) but the r e p r o d u c i b i l i t y was not very good. The d i f f e r e n c e i n r e s u l t s may have been due t o contamination at the end of Run 53 and the p o s s i b l e surface c o n d i t i o n change of the nozzle as a r e s u l t of the flaming. P r i o r t o Run 66 i n which methyl i s o b u t y l ketone flowed out of the 3/16 i n . I.D. brass nozzle i n i n t e r m i t t e n t a n d i i r r e g u l a r spurts of m u l t i p l e drops, s i n g l e drops without t r a i l e r s were considered t o be uniform i n s i z e . This u n i f o r m i t y was evidencedby the v i s u a l o b s e r v a t i o n of the drops and v i s u a l i n s p e c t i o n of the movie f i l m taken. However, jLcia of the regions of single drops obtained i n plots of volume per stroke against pump strokes per second show d e f i n i t e shape trends, but vary considerably i n actual shape and s i z e . This f a c t , together with the i r r e g u l a r and intermittent spurts of methyl i s o b u t y l ketone when disbursed into water through a 3/16 i n . I i D . brass nozzle, suggest that the drop size of single drops without t r a i l e r s may not be as uniform as previously considered. Consequently, the word "uniform" has not been used when describing single drops without t r a i l e r s . To provide a permanent record some 150 feet of 16 mm f i l m was filmed at 16 and 64 frames per second with the Bolex Camera, and processed negative. S t i l l photographs were taken throughout each run with the 35 mm Exakta Camera. Unfortunately the s t i l l photographs of runs 58 to 64 i n c l u s i v e were l o s t as a resu l t of a camera defect i n the Exakta Camera. A l l the negatives of the aboveIphotographs are f i l e d with the Department of Chemical Engineering. 112 CONCLUSION The p r o d u c t i o n o f s i n g l e drops w i t h o u t t r a i l e r s u s i n g t h e p e r i o d i c i n j e c t i o n system t e c h n i q u e o f t h i s i n -v e s t i g a t i o n r e q u i r e d t h a t t h e f o l l o w i n g c o n d i t i o n s be f u l f i l l e d . 1. C o r r e c t n o z z l e s i z e . The n o z z l e t i p i n s i d e d i a m e t e r was v e r y c r i t i c a l f o r s i n g l e drops t o be formed i n systems o f v e r y low i n t e r f a c i a l t e n s i o n . T i p d i a m e t e r appeared l e s s c r i t i c a l i n systems o f h i g h e r i n t e r f a c i a l t e n s i o n . 2. S i n g l e drops were formed o n l y when t h e n o z z l e t i p was not w e t t e d by t h e d i s p e r s e d phase. W e t t a b i l i t y was a f f e c t e d by ~ (a) n o z z l e m a t e r i a l (b) n o z z l e d i a m e t e r ( c ) s u r f a c e a c t i v e c o n t a m i n a n t s . 3« The volume p e r d r o p , and t h e pump s t r o k e s p e r second had t o be w i t h i n s p e c i f i e d l i m i t s f o r each n o z z l e s i z e and system. 4. B o t h t h e t e m p e r a t u r e o f t h e system, and t h e v e l o c i t y t i m e p r o f i l e o f t h e d i s p e r s e d phase i n t h e n o z z l e as s t u d i e d w i t h d i f f e r e n t cam shapes, a f f e c t e d t h e a r e a s o f s i n g l e u n i f o r m drops on p l o t s o f volume p e r s t r o k e a g a i n s t pump strokes per second. However these f a c t o r s were l e s s important than those i n items 1 t o 3 above. SUGGESTIONS FOR FURTHER STUDY This i n v e s t i g a t i o n was l i m i t e d t o two systems of low i n t e r f a c i a l t e n s i o n , three nozzle m a t e r i a l s , and c y l i n d r i c a l l y bored sharp edged n o z z l e s . The f o l l o w i n g suggestions are submitted f o r a f u r t h e r study of the problem. 1. Accurate drop s i z e measurements should be made t o study the u n i f o r m i t y of the s i n g l e drops without t r a i l e r s . These measurements could be made from the 16 mm movie f i l m s of s i n g l e drops without t r a i l e r s taken during t h i s research and f i l e d w i t h the Department of Chemical Engineering. However more accurate determinations of drop s i z e could be obtained from photographs taken w i t h the 35 mm Exakta Camera of s i n g l e drops at s u f f i c i e n t height above the nozzle f o r the o s c i l -l a t i o n s from drop formation t o have die d out. 2. Other l i q u i d systems of d i f f e r e n t i n t e r f a c i a l t e n s i o n should be examined t o f i n d the e f f e c t of i n t e r f a c i a l t e n s i o n on the production of uniform drops w i t h v a r i o u s l y s i z e d n o z z l e s . 3. Other nozzle m a t e r i a l s should be t e s t e d , ranging from h y d r o p h i l i c t o hydrophobic i n nature. 4. The cam operated a d j u s t a b l e stroke mechanism s u f f e r s from considerable wear. I t i s suggested t h a t t h i s be r e b u i l t i n c o r p o r a t i n g the present design w i t h the f o l l o w i n g mod-i f i c a t i o n s : ia}0 (a) the body be e i t h e r m i l l e d from one piece of bra s s , or constructed w i t h a c c u r a t e l y machined j o i n t s and made r i g i d . (b) replaceable bushings be used f o r the cam f o l l o w e r and stroke arm rod bearings. (c) the moveable fulcrum be operated i n a s l i d e so t h a t there i s no l a t e r a l t h r u s t c a r r i e d by the adjustment screw. 5. The Hoke valve used as a pump be replaced permanently by the bellows pump. The s t i f f n e s s of the bellows s p r i n g i n the Hoke bellows valve pump caused most of the wear i n the cam actuated v a r i a b l e stroke mechanism. Il6< APPENDIX A Sizes of Brass Nozzles Used'. Nominal i n s i d e Measured i n s i d e diameter i n . . diameter (by-t r a v e l l i n g microscope) cm. i n . 1/8 0;323 6.127 5/32 0.15$ l l / 6 > o.ms 0.177' l l / 6 1 f (Run 52 only) 0.179 3/167 0.189 I 1 1 7 APPENDIX B Surface Tension and I n t e r f a c i a l Tension Measurements at 69°F M a t e r i a l Surface Tension I n t e r f a c i a l dynes per Tension dynes cm. per cm. ~ D i s t i l l e d water 7 7 . 1 n-Butanol (tech) 2 7 . 5 n-Butanol and water ' 2 . 4 Methyl I s o b u t y l Ketone 2 6 . 9 Methyl I s o b u t y l Ketone and water 6.9 118 REFERENCES Hayworth, C.B., and T r e y b a l , R.E., Ind. Eng. Chem. 42, 1174, (1950) K e i t h , F.W., and Hixson, A.N., Ind. Eng. Chem. 47., 258.(1955). -Lewis, J.B., Jones, I . , and P r a t t , H.R.C., Trans. I n s t . Chem. Engrs. (London), 2£, 126 (1951). Fujinawa, K., Maruyama, T., and Nakaiko, Y., Chem. Eng. (Japan) 21, No. .4.,. 194 (1957). Siemes, W., and Kauffmann, J.F., Chem.-Ing.-Tech., 1, 32 (1957). Tanweer, A.K., J o u r n a l of the I m p e r i a l College Chemical Engineering S o c i e t y , _10, 51 (1956). J o s h i , J . D., Ph.D. T h e s i s , U n i v e r s i t y of London (1951). N u l l , H. R., and Johnson, H.F., A.I.Ch.E. J o u r n a l , 4, No...3, 273 (1958). . . . Kl e e , A.J., and T r e y b a l , R.E., A.I.Ch.E. J o u r n a l , 2, 444 (1956). . Hu, S., and K i n t n e r , R.C., A.I.Ch.E. J o u r n a l 1, 42 (1955). Johnson, A.I.. and B r a i d a , L.., Can. J . Chem. Eng., 165 (1957). E l z i n g a , E.R., and Banchero, J.T., A.I.Ch.E. J o u r n a l 1, No. 3, 394 (1961). Rodger, W.A., T r i c e , V.G., and Rushton, J.H., Chem. Eng. Prog., ^ 2 , No. 12, 515 (1956). . . Davies, J.T., Trans. I n s t . Chem. Engrs. (London), 38, 289 (I960). . . . . 119 15. Buchanan, R.H., Aus. J . Appl. S c i . , 3 , 233 (1952). 16. R o c c h i n i , R.J.., M.A.Sc. Th e s i s , U n i v e r s i t y of B r i t i s h Columbia, (1961). 17. Cavers, S.D., and Ewanchyna, J.E., Can. J . Chem. Eng., 113 (1957). 18. Coulson, J.M. > and Skinner, S.J., Chem. Eng. S c i . , 1, No. 5/197 (1952). 19. Sharkey, W.A., B.A.-Sc. T h e s i s , U n i v e r s i t y of B r i t i s h Columbia ( i 9 6 0 ) . 20. Greene, R.A., BiA.Sc. T h e s i s , U n i v e r s i t y of B r i t i s h Columbia, (1961). 21. Thompson, D.W., Trans. I n s t n . Chem. Engrs, 39, 289 (1961). FIGURE I " O B L A T E SPHEROID DROP" SHAPE ( TWO CONJOINED O B L A T E SEMI SPHEROIDS ) A H B o M GENERAL LAYOUT ELECTRIC COUNTER CIRCUIT of t J "6 ELECTRONIC FLASH CIRCUIT * — 0 FIGURE 3 DIAGRAMMATIC LAYOUT OF APPARATUS PRELIMINARY INVESTIGATION ^ 3 6? hGZ F I G U R E 4 OPTICAL ARRANGEMENT PRELIMINARY INVESTIGATION ^ 5 £7 SCALE* 3" = r-Oa p63£7 IO o o 6 r bearing used as a follower wheel. Light press fit with f- Departure R2 ball BEARING POST S c a l e : Twice Size No. 5 0 Drill, 2 - 5 6 U N C - 2 B £ Drill x | deep ROD CAP Scale '• Twice Size 28 U N - 2 B I B I long; 2 holes V A L V E H O L D E R S c a l e : Full Size F I G U R E 7  P U M P DRIVE COMPONENTS S C A L E S A S SHOWN F I G U R E 9 C A M F O L L O W E R SCALE * TWICE-"SIZE F IGURE 10 CAM "A" SCALE : 4 x SIZE COLLI MATED LIGHT FROM FRESNEL LENS 1 1/2" WIDE S L H \ 4 ^RED CELLOPHANE FILTER APPARATUS PANEL REAR ADJUSTABLE MIRROR ' FRONT ADJUSTABLE MIRROR CAMERA SCALE« 1/2 SIZE F I G U R E 14 REVISED MIRROR ARRANGEMENT lg Brass No. 36 Drill No. 6 - 3 2 U N C - 2 B • i — -— K M - I CM Place | - I 6 U N C - 2 B nut ft washer on post before soldering top. | - I 6 U N C - 2 A 23 d , 32 MIRROR H O L D E R i " 16 B r 0 8 8 row) 2 • HOLDER STRIP FIGURE 15 PORTABLE MIRROR HOLDERS S C A L E : FULL SIZE 3 * $ LL. 40 10 i o 30 al 2* o ac o>20 ui 5 =J _ l O > I 0 LEGEND MINIMUM VALUES FOR g I DROP a I TRAILER 6 I DROP 6 2 TRAILERS •O I DROP 8 3 TRAILERS O- BOUNCE I DROP A I LARGE TRAILER 9—B—9-M U L T I P L E DROPS "9" 3L 0 E R R A T I C - I DROP 0 , V — p ~ ° — ° ~ a I TRAILER / S T R O K E M 0 " / « , 0-50 1 0 0 1-50 P U M P STROKES / S E C . FIGURE 17 RUNS 14-24 TYPES OF DROPS PRODUCED 1/8" STAINLESS STEEL NOZZLE CAM"A" FORWARD n-BUTANOL and WATER 2 0 0 3 t $ Oo LEOENO 50 H ro ^ 4 0 30 ui O tc I -2 20 o > 10 O Q + » t 2 3 DROP 8 0 TRAILER DROP & I TRAILER DROPS & I TRAILER DROPS a I TRAILER LIMIT OF APPARATUS ^ • 5 I DROP a I TRAILER ERRATIC - I DROP |0 H a I TRAILER / » 0 H | / STROKE 0 50 100 PUMP STROKES FIGURE 18 / SEC. 1-50 RUN 35 TYPES OF DROPS PRODUCED AND REGION OF SINGLE DROPS 5/32" I.D. STAINLESS STEEL NOZZLE CAM "A" REVERSED n-BUTANOL ond WATER 2 0 0 PUMP STROKES / SEC. FIGURE 19 R U N 38 TYPES OF DROPS PRODUCED AND REGION OF SINGLE DROPS 5/32" I.D. BRASS NOZZLE CAM V FORWARD nrBUTANOL and WATER AO vQ O Ci 0 n " 0 11 / " - J . L : I L -0-50 I 0 0 1 5 0 2 0 0 PUMP STROKES / SEC. FIGURE 20 R U N 3 9 T Y P E S O F DROPS PRODUCED AND REGION O F SINGLE DROPS 5 / 3 2 " I.D. B R A S S N O Z Z L E C A M "A" R E V E R S E D n - B U T A N O L and W A T E R L E G E N D O O m X> I DROP a 0 TRAILER 1 DROP a I TRAILER 2 DROPS a I T R A I L E R MORE T H A N I DROP LIMIT OF APPARATUS I D R O P a I T R A I L E R ERRATIC 'T I DROP a I TRAILER / S T R O K E Q H | " 0 " / "j 0 50 100 1-50 P U M P S T R O K E S / S E C . FIGURE 2| RUN 40 T Y P E S O F DROPS P R O D U C E D AND REGION O F SINGLE DROPS 5 / 3 2 " ID . B R A S S N O Z Z L E C A M "A" F O R W A R D , 1/4" S P A C E R n - B U T A N O L and W A T E R 2 0 0 L E G E N D O I DROP a O TRAILER 9 I DROP a I TRAILER LIMIT OF APPARATUS * 2 DROPS & I TRAILER ERRATIC - I DROP a I T R A I L E R / S T R O K E I 0 | I I n 0 I I / | n | 0 50 100 I 50 200 PUMP S T R O K E S / S E C . FIGURE 22 R U N 41 T Y P E S O F DROPS PRODUCED AND REGION OF SINGLE DROPS 5 / 3 2 " I.D. B R A S S N O Z Z L E C A M " B " n - B U T A N O L and W A T E R fr to 4 o 50 4 0 3 0 o cr 20 5 10 L E G E N D O I DROP & 0 TRAILER P I DROP a I TRAILER 4 2 DROPS a I TRAILER 0 3 DROPS a I TRAILER \5 MORE THAN I DROP 3 B R 0 P S aiTRAILER L IMIT OF APPARATUS D R O P a I T R A I L E R -<? ERRATIC- I DROP a I T R A I L E R / S T R O K E X JL 0-50 I 00 PUMP I 50 STROKES / SEC. F I G U R E 2 3 R U N 4 2 T Y P E S O F DROPS PRODUCED AND REGION O F SINGLE DROPS 5 / 3 2 " I.D. BRASS N O Z Z L E CAM "A" FORWARD (REPAIRED) n - B U T A N O L and W A T E R 2 0 0 LEGEND 9 I DROP & I TRAILER 6 I DROP a 2TRAILERS -O I DROP a 3 TRAILERS O BOUNCE 4 2 DROPS a I TRAILER MULTIPLE DROPS 2 °*0PS NO MULTIPLE DROPS 2 T R A I L E R S / DROP -6-^R^LERS/DROP-2 T R A I L E R S / DROP 6 6 ° " I T R A I L E R / DROP I E R R A T I C - I DROP ft I TRAILER / S T R O K E 0^ H H 0 I I \ / II 0 5 0 1 0 0 I 50 PUMP S T R O K E S / S E C . FIGURE 24 RUN 43 TYPES OF DROPS PRODUCED 1/8* I.D. BRASS NOZZLE CAM "A"FORWARD n-BUTANOL and WATER 2 0 0 o o so LEGEND I DROP 8 I TRAILER I DROP a 2 TRAILERS 1 DROP ft 3 TRAILERS BOUNCE 2 DROPS a TRAILERS 3 DROPS a TRAILERS ro 6 e 4 0 U i 3 0 o OC w 20 s -J O > 2 TRAjLERS/DROP 2 OROPS a TRAILERS ~ • OROP • > 10 -ERRATIC- I OROP a I TRAILER / STROKE 0 " » 0 •• / n I I X 0-50 I 00 1-50 PUMP STROKES / SEC FIGURE 25 RUN 4 4 TYPES OF DROPS PRODUCED 1/8 w I.D. BRASS NOZZLE CAM "A" R E V E R S E D n-BUTANOL and WATER 2 0 0 ^ 3 te~7 ro '6 4 0 3 0 •O O LE6END I DROP & I T R A I L E R 1 DROP a 2 T R A I L E R S I DROP a 3 T R A I L E R S B O U N C E . o £ 2 0 co Ul 2 3 _ l O > i o 3 TRAILERS / DROP E R R A T I C - I, D R O P a I T R A I L E R / S T R O K E 0 " " 0 " / u X X 0 50 0 0 1-50 PUMP STROKES / S E C . 2 0 0 F I G U R E 2 6 RUN 45 TYPES OF OROPS PRODUCED 3/16" LD. BRASS NOZZLE CAM " B " n- BUTANdL and WATER L 0 ? S ro i O 4 0 -e 30 ' Ul o £ 20 to Ul 3 .o o > LEGEND I D R O P ft I T R A I L E R I DROP ft 2 T R A I L E R S I OROP a 3 T R A I L E R S I D R O P a 4 TRAILERS B O U N C E I TRAILER / DROP £b O "0* / — B O U N C E I T R A I L E R / DROP p— E R R A T I C - (I DROP a I T R A I L E R / S T R O K E 0 » •* 0 <• / •• I l _ 0-50 1 0 0 P U M P S T R O K E S / SEC 1-50 FIGURE 27 TYPES OF DROPS PRODUOED 3/16" I.D. BRASS NOZZLE CAM W. FORWARD n-BUTANOL and WATER RUN 46 P7 L E G E N D Q I DROP a I T R A I L E R 6 I DROP a 2 T R A I L E R S -O I DROP a 3 TRAI L E R S O- B O U N C E o&o? 2 T R A I L E R S / D R O P BOUNCE 0 -TRAILER / DROP -Q _ 9 _ ERRATIC I DROP a I T R A I L E R / S T R O K E ± 0 5 0 100 I 50 PUMP S T R O K E S / S E C FIGURE 28 RUN 47 T Y P E S O F DROPS PRODUCED 3/16" I.D. B R A S S N O Z Z L E CAM 'W REVERSED n - B U T A N O L and W A T E R 2 0 0 hi LEGEND 8 I DROP a I TRAILER I DROP a 2 TRAILERS -O I DROP a 3 TRAILERS O B O U N C E -Q—. 2 TRAILERS / DROP 2 . T R A I L E R S / . DROP - -6— -O-I T R A I L E R / DROP - o B O U N C E f > — •9-T R A I L E R / DROP - 9 -V E R R A T I C - 1 DROP a I T R A I L E R / S T R O K E Q M II Q II / II -I I -o--9-0 5 0 100 1-50 PUMP S T R O K E S / SEC FIGURE, 35 TYPES OF DROPS PRODUCED II / 64 w I.D.TEFLON NOZZLE CAM 'W FORWARD n-BUTANOL and WATER RUN 48 2 0 0 LEGEND ro i O 4 C -S -O o I DROP a .1 TRAILER I DROP a 2 TRAILERS I DROP a 3 TRAILERS BOUNCE i 3 C -ui • * o ce (0 v . Ul s _l O > 2 0 -9-2 TRAILERS / OROP - 6 6--o ERRATIC -I TRAILER / DROP I TRAILER / DROP <? "Q-I DROP 8 I TRAILER: / STROKE 0 II n 0 " / " X 0 50 •00 150 PUMP STROKES / SEC F I G U R E 3 6 TYPES OF DROPS PRODUCED 11/64" I.D. TEFLON NOZZLE CAM 'A" REVERSED n-BUTANOL and WATER RUN 49 -6-BOUNCE _o 2 0 0 co p ^ 50 -io 2 40 ui 30 o OC W 5 20 -10 . RUN 40 FIGURE 2:1 RUN 42 FIGURE 23 / \ / \ 2 DROPS a I TRAILER I DROP & I TRAILER ERRATIC-1 DROP a I TRAILER c / STROKE 0 II H o " - I " J L 050 100 1-50 PUMP STROKES/ SEC F IGURE §5 EFFECT OF CAM SPACER FIGURES 2t a 23 SUPERIMPOSED n-BUTANOL and WATER 2-00 sr ERRATIC — I DROP 8 1 T R A I L E R / STROKE i 0 » » 0 | * / * t , 0 0-50 1 00 I-SO 2-00 PUMP STROKES/ SEC F I G U R E §4 STAINLESS STEELS BRASS NOZZLES FIGURES 18 a 20 SUPERIMPOSED n-BUTANOL an* WATER ft 

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