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The removal of smokes and mists Guthrie, David Alan 1955

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THE REMOVAL OF SMOKES AND MISTS by DAVID ALAN GUTHRIE  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 to the standard required from candidates f o r the degree o f MASTER OF APPLIED SCIENCE.  Members o f the Department o f Chemical Engineering  THE UNIVERSITT OF BRITISH CODJMBIA September, 1955  ABSTRACT A coloriiaetric quantitative analysis f o r di-n-octylphthalate and other aromatic esters has been developed which i s capable o f determining as l i t t l e as 0.1 milligrams o f an e s t e r .  This method i s based on the forma-  t i o n o f hydroxamic a c i d from esters using hydroxylamine hydrochloride i n an alkaline medium. On the addition o f an a c i d i f i e d solution o f f e r r i c p e r chlorate, a red-colored complex o f f e r r i c hydroxamate i s formed, proportion ate  i n i n t e n s i t y to the weight o f ester present. Mist composed o f di«*i-octylphalate  droplets of  0.869 microns  average diameter was removed from a i r at s u b s t a n t i a l l y atmospheric temperature and pressure by passing the a i r up through a bed o f 150/200 mesh s i l i c a g e l f l u i d i z e d i n a 2-1/U  inch glass column.  Removal e f f i c i e n c y , de-  f i n e d as the percent (by weight) removal of the mist was s u b s t a n t i a l l y i n dependent of the entering concentration over the range milligrams of ester per cubic foot o f a i r .  For a given bed, removal e f f i c i  ency improved with decreasing s u p e r f i c i a l gas v e l o c i t y . were used, 13.25  0.765 t o 0.965  grams per square centimeter and  25.35  Two bed weights grams per square  centimeter, and i t was found that the removal e f f i c i e n c y was p r a c t i c a l l y i n dependent o f the bed weights. The maximum removal e f f i c i e n c y was a s u p e r f i c i a l bed v e l o c i t y of 3.2 of 13.25  88.8$ at  centimeters per second and a bed weight  grams per square centimeter. The same mist was removed by passing the gas stream through  various v e n t u r i nozzles with ports i n the throat through which f i n e s i l i c a gel  (150/200 mesh) entered by g r a v i t y and a s p i r a t i o n into the gas stream.  For  the v e n t u r i nozzles the removal e f f i c i e n c y generally increased with  increasing v e l o c i t i e s ; however, the maximum removal e f f i c i e n c y obtained was only about  z that I t i s shown/the behavior and c o l l e c t i o n e f f i c i e n c e s obtained with the two devices can be s a t i s f a c t o r i l y explained i f the f l u i d i z e d bed i s assumed to c o l l e c t the aerosol p a r t i c l e s by d i f f u s i o n a l processes only, and the v e n t u r i tube, by i n e r t i a l processes only, at l e a s t f o r aerosol p a r t i c l e s of the size used i n t h i s work. The problem of e f f i c i e n t removal of aerosol p a r t i c l e s i n t h e range of 0,1 to 1.0 microns diameter has s t i l l not been solved i n an economical manner f o r many cases of i n d u s t r i a l importance.  The removal becomes even more  d i f f i c u l t when the aerosol p a r t i c l e s are f a i r l y uniform i n s i z e . The purpose of the present work was t o conduct a preliminary t e s t i n g of new devices which might be more e f f i c i e n t f o r small p a r t i c l e s than those now commonly used.  TABLE OF CONTENTS  ABSTRACT  1  INTRODUCTION AND THEORY  3  EXPERIMENTAL APPARATUS  9  PROCEDURE  13  RESULTS  16  DISCUSSION OF RESULTS  k9  SUMMARY  55  NOMENCLATURE  57  BIBLIOGRAPHY  58  DATA AND CALCULATIONS  59  APPENDICES  79  ,  3  INTRODUCTION AND THEORY The problem o f the removal o f dispersoids from gas streams Is not a new problem, but because/relatively recent l e g i a l a t i o n more money and time are  being spent to f i n d economical methods o f preventing atmospheric p o l l u t i o n .  Many industries have made the sale o f the products stripped from the stack gases pay f o r the removal c o s t s .  For example, the Consolidated Mining and  Snelting Company at T r a i l , B. C , has b u i l t a f e r t i l i z e r d i v i s i o n to u t i l i z e #  the  sulfates and s u l f u r i c a c i d produced from the s u l f u r dioxide removed  from exhaust gases from t h e i r m e t a l l u r g i c a l p l a n t s . Before any experimental work can be done i n dust removal, i t i s necessary to have a suitable source o f smoke or mist and to have a method for determining the concentration o f p a r t i c l e s i n the gas stream.  To ob-  t a i n the data f o r t h i s report a homogenous aerosol was produced using apparatus s i m i l a r t o that reported by LaMer and S i n c l a i r (6-7-18). The operation o f the LaMer - S i n c l a i r generator i s based on the p r i n c i p l e o f c o n t r o l l i n g droplet s i z e by slow cooling o f a vapour i n the presence o f a r t i f i c i a l n u c l e i .  Clean, dry a i r i s f i r s t passed over a heated  nichrome wire, previously coated with sodium chloride, and then i n t o a vaporizer.  This a i r contains minute c r y s t a l s of sodium chloride and these  can serve as condensation n u c l e i .  The generating substance (which i n t h i s  case was di-n-octylphthalate) i s heated i n the vaporizer at a constant temperature.  The clean, dry a i r i s passed through the l i q u i d at a steady  flow to saturate i t with vapor.  This mixture of a i r , vapor and n u c l e i i s  then passed i n t o a reheater which i s kept at a higher temperature than the vaporizer i n order t o ensure that a l l the generating material i s i n the vapor state. cooled.  The mixture i s next passed into a v e r t i c a l chimney where i t i s slowly Upon cooling, the vapor becomes s l i g h t l y supersaturated and drop-lets con-  4-  tinue to grow while r i s i n g i n the column by a process of d i f f u s i o n .  The  t h e o r e t i c a l aspect of the growth process has been discussed by Reiss  and  La Mer.  (I4). The method f o r determining the concentration of aerosol i n the  gas stream was modified from a method reported by H i l l (U,50 analysis of a l i p h a t i c e s t e r s .  f o r the  The q u a l i t a t i v e spot tests f o r carboxylic  acids and esters are the basis f o r t h i s method. When an ester i s warmed i n an a l k a l i n e media with hydrox<pl4mine hydrochloride, hydroxaraic a c i d i s formed. F i e g l (1) reports the following RCOOR  •  equations:  NH OH •  RCO(NHOH)  z  *  ROH  F e r r i c i r o n forms a b r i g h t red or lavender complex with hydroxamic acids i n a c i d media according to the r e a c t i o n : RCO(NHOH)  +  Ft"  »  H R-C "? N  The red complex i s r e a d i l y soluble i n aqueous ethanol. This method has not previously been reported f o r the of aromatic e s t e r s .  determination  This i n v e s t i g a t i o n shows i t to be a u s e f u l and sensitive  method for the quantitative determination  of esters such as benzoates and  phthalates. Lapple (8) states that performance of a dust c o l l e c t o r i s termed c o l l e c t i o n e f f i c i e n c y and i s generally expressed as a weight r a t i o o f dust (or mist) c o l l e c t e d to weight of dust entering the apparatus.  According  t h i s d e f i n i t i o n c o l l e c t o r e f f i c i e n c y i s i n i t s e l f not a s p e c i f i c  to  character-  i s t i c of a given c o l l e c t o r , but depends on operating conditions as w e l l as on the p h y s i c a l properties of the p a r t i c u l a r dust treated. Perry ( l l ) c l a s s i f i e s gas dispersoids as: Mechanical dispersoids Dust  - p a r t i c l e diameter greater than 1 micron.  Spray - p a r t i c l e diameter greater than 10 microns.  s Condensed dispersoid Fume - particle diameter less than 1 micron. Mist - particle diameter less than 10 microns. For the sake of simplicity the.terms "dust" and "mist" will- arbitrar i l y be used to describe any solid or liquid dispersoid respectively. Perry (11) and Lapple (8) l i s t the following forces or mechanisms u t i l i z e d i n the design of a i r purification equipments 1.  Sonic  2.  Thermal  3.  Electrostatic  li.  Gravitational  £ • Physio chemical 6.  Filtration  7.Inertia! Since the f i r s t four do not concern this report, i t i s suggested that anyone interested in these refer to the references mentioned. Just exactly which mechanism governs dust or mist removed i s dependent to a very great extent on the dispersoid particle size.  Suitable equipment  has been designed to remove particles of 5 microns diameter or larger; however, this equipment has been found to be unsuitable when used to remove particles of less than 1 micron diameter, particularly as the particle size becomes more uniform.  To emphasize this point Wilson (18) has recently reported on a  turbo-cyclone which reports efficiencies of over 90$ for heterogeneous aerosols of O J . to 10 microns diameter. When a homogeneous aerosol of 0.5 microns diameter was treated i n the same apparatus, efficiencies reported were considerably less than $0%. The cyclone mentioned i n the preceding paragraph i s an example of one of the many pieces of equipment which have been designed on the basis that inertia! forces w i l l effect the removal.  The underlying principle of the  6  i n e r t i a ! mechanism i s that when a dust laden f l u i d flows towards a body, the f l u i d w i l l be deflected around the body whereas the dust particles by virtue of this greater inertia w i l l pass through the laminarr boundary layer arid impinge; on the collecting surface.  Since both mass and velocity have  an effect on the inertia of a body, both of these factors must be considered in the design of inertial type equipment. Collection of aerosol particles by inertial mechanisms has been discussed by Langmuir and Blodgett (9). They state that the collection efficiency i s described by a target efficiency which represents the fraction of particles i n the f l u i d volume swept by the body which w i l l impinge on the body. This target efficiency, function of the dimensionless group, U.^ Vo g "Dp  Vf ^*  ^  , is a  , where  = terminal velocity of the aerosol particle average velocity of the f l u i d - acceleration of gravity - diameter of the collecting body  Curves showing the relationship between the target efficiency and the dimensionless group have been drawn by the above authors for targets of various shapes. High collection efficiences (90%) by inertial means can only be expected i f the value of the dimensionless group i s 0.5 or more. Below this value collection efficiency decreases rapidly.  A further discussion of  i n e r t i a l mechanisms i s given by Wong et a l (19,20); however, much of his work as reported i s beyond the scope of this report. One of the most common methods of dust removal i s f i l t r a t i o n . industries have installed bag houses and use cloth f i l t e r s (12).  Many  A great  many of the so-called dust f i l t e r s remove dust because of some other mechanism, for example, the common fibre f i l t e r used i n many homes i s actually a combined f i l t e r and inertial-type separator.  Another common type of f i l t e r i s  7 the coke f i l t e r used i n the s u l f u r i c a c i d industry and i n t h i s case p a r t i c l e c o l l e c t i o n i s attributed i n part to d i f f u s i o n a l mechanisms;. The collection, of aerosol p a r t i c l e s by d i f f u s i o n a l mechanisms i s known to be of importance for p a r t i c l e s o f 1 micron diameter or l e s s and i s the most important mechanism f o r droplets o f less than 0.1 microns diameter. The s t a t i s t i c a l average l i n e a r displacement A S o f a p a r t i c l e i n  y  any given d i r e c t i o n i s given by the equation  4RTfc™t ~  where R  Gas constant  T  Tamperature  kjn  Cunningham correction factor f o r Stoke »s Law  t  Time  Vtl  Fluid viscosity  N  Avagadro's number  Dp  P a r t i c l e diameter  For f i x e d experimental conditions using a homogeneous aerosol, the d i s p l a c e ment o f a p a r t i c l e because o f Brownian motion should be a function o f time only. Values f o r t h e Cunningham correction factor to Stoke»s Law, which allows the c a l c u l a t i o n of terminal v e l o c i t i e s and d i f f u s i o n a l displacements have been given by Lapple, ( 8 ) . The coke f i l t e r , which has already been mentioned, i s an example o f a f i x e d bed.  A f i x e d bed i s one i n which each p a r t i c l e has a f i x e d  position r e l a t i v e to every other p a r t i c l e and to the walls of the container; whereas a moving bed, which has been used f o r smoke removal (13), i s one i n which each p a r t i c l e remains f i x e d r e l a t i v e to the other p a r t i c l e s but  8 moves; with respect to the w a l l s . A t h i r d type o f bed, a f l u i d i z e d bed, i s one i n which each p a r t i c l e moves r e l a t i v e to every other p a r t i c l e and to the w a l l a l s o .  I t i s important to note that the f l u i d i z e d bed has a def-  i n i t e upper boundary and i n t h i s respect d i f f e r s from a f l u i d - s o l i d transport stream.  Although no i n d u s t r i a l use o f t h e f l u i d i z e d bed f o r smoke removal  has been reported, t h i s type o f bed has c e r t a i n advantages. pressure drop through a i 1.„!..' r  For example, the  bed increases with v e l o c i t y up to a c e r t a i n  point only, beyond which the pressure drop i s p r a c t i c a l l y constant.  More-  over t h i s pressure i s small compared to pressure drops through turbo-cyclones and v e n t u r i scrubbers.  I t i s possible with both the moving and f l u i d i z e d  beds to remove o l d s o l i d s and to add new s o l i d s continuously, but again because o f the turbulence within the f l u i d i z e d bed t h i s bed has the advantage of being able to r e t a i n more aerosol before needing r e p l a c i n g .  The  appar-  atus f o r the f l u i d i z e d bed i s much simpler to construct than are cyclones and yet  the absorbed material can be removed and the absorbate reused, a factor  which could prove to be e«onomically important. Meissner and Mickley (10) have reported that mists composed of s u l f u r i c acid droplets 2 to l l | microns i n diameter were f i l t e r e d from a i r using f l u i d i z e d beds of various non-porous and porous m a t e r i a l  The  porous bed had a r e l a t i v e l y short l i f e , whereas the porous beds, l i k e gel,  could absorb %  t  nonsilica  by weight, before s t i c k i n g destroyed f l u i d i z a t i o n .  They found that removal e f f i c i e n c y was s u b s t a n t i a l l y constant during the l i f e of •the beds and independent o f the entering concentration over the range o f from 20 to 120 pounds of a c i d (100$ basic) per 1,000,000 cubic f e e t . For a given f l u i d i z e d bed, removal e f f i c i e n c y improved with increasing superf i c i a l gas v e l o c i t y and with increasing bed weight per u n i t area.  Meissner  s$A Mickley (10) proposed that t h e removal was affected by i n e r t i a l mechanisms and thus explained the improvement o f c o l l e c t i o n e f f i c i e n c y with i n -  1 creased v e l o c i t i e s .  They proposed the  equation  where U  0  s u p e r f i c i a l gas v e l o c i t y  Ci  i n l e t concentration  C2  outlet concentration  k  constant  W n  bed weight per unit area constant  EXPERIMENTAL APPARATUS: The equipment required f o r the a n a l y t i c a l work consisted of t wo water baths complete with thermoregulators,  mixers, heaters, and thermometers.  A K l e t t - Summ§r-sgn photo-electric colorimeter was used to measure transmission i n the edi-octylphthalate determination. stant voltage  This imet'exd was  connected to a con-  transformer.  The construction of the homogenous aerosol generator was a design described by LaMer (6). on page it© .  The vaporizer was  ameter and 30 cms. deep.  A schematic sketch of the apparatus i s shown  a glass c y l i n d e r approximately  8 cms.  in di-  The rehedferwas a round-bottomed two l i t e r f l a s k .  The chimney, a double-walled ground glass j o i n t s .  based on  condensor, was f i t t e d into the reheater using  The enucleation chamber was  a sphere of l£ cms.  diameter  equipped with a support rod and a grounl glass j o i n t f o r the nichrome heating coil.  This nichrome c o i l was made from 127  t o t a l resistence.  gage wire and had about 10 ohms  The c o i l was s i l v e r - soldered to two tungston  contacts  which passed through and were sealed i n the male end of the ground glass joint.  The power was supplied from a constant voltage -transformer. The a i r baths suggested by LaMer (6) were iglaced with two  stainless  DOUBLE-WALL  HOSE  CHIMNEY  E.M. F.  -  SAMPLER OL A S 8 COLUMN MANOMETERS  WET-TEST  METER  TUBINO  FIGURE  DEPT. O F CHEM. ENO. U.  B.  C  SCHEMATIC OF  THE  I  SKETCH APPARATUS  DAVID. A JULY  GUTHRIE  12 1 9 5 3  II  s t e e l tanks each containing  bath wax*  heated by two immersion heaters  These baths were regulated and were  operating i n p a r a l l e l through a v a r i a c .  Each  bath was also equipped with a visible speed s t i r r e r and two thermometers located at separated points i n the bath. The a i r used was the b u i l d i n g supply.  I t passed f i r s t through a  pressure control valve and then through two drying tubes and two f i b r e - g l a s s f i l t e r i n g tubes.  At t h i s point the a i r flow was divided and part of the flow  passed through a meter into the m u c l e a t i o n chamber. a i r was metered i n t o the preheater, an  The other part of t h e  8 mm. glass c o i l immersed i n the  bath, and then passed down through the long tube of the vaporizer. A l l a i r flow meters were c a p i l l a r y tubes which acted as ori'fiees. The pressure drop across these tubes was measured using manometers. Manometers were also i n s t a l l e d to measure the absolute pressure on the i n l e t side of a l l c a p i l l a r i e s .  The rnucleation chamber, preheater, and reheater  f l a s k were a l l connected t o the vaporizer using glass b a l l and socket j o i n t s . The a i r l i n e s from the valve to «W» where the a i r enters the generator, the bleed-off l i n e , and the d i l u t i o n flow l i n e were a l l 8 mm. i n diameter.  From  the top of the chimney through to the wet-test meter 17 mm. tubing was used. The. l i n e from the chimney was connected to the 2| inch glass column used f o r 5  the f l u i d i z e d bed,by a 2 inch brass reducing coupling.  The bed material was  1^0/200 T y l e r mesh s i l i c a gel supported on a 200 mesh screen.  Manometers  were i n s t a l l e d to measure the i n l e t pressure t o the bed and to measure the pressure drop across the bed. The a i r flow could be directed along three paths.  I t could by-pass the column, pass through the column and by-pass the  sampler, or pass through the column and through the sampler into the wett e s t meter.  The f i l t e r used to sample f o r aerosol concentrations i n a l l  streams was a MF f i l t e r (3). I t i s sometimes referred to a s a m i l l i p o r e filter.  I t i s not t r u l y a paper, but i s a c t u a l l y a sheet of c e l l u l o s e e s t e r s .  12 I t i s about 15>0 microns thick and has a t o t a l pore volume equal t o 80% t o 8$%. I t i s supposedly insoluble i n petroleum ether; however the ether destroys the c e l l structure.  The greatest disadvantage of these f i l t e r s  i s the  cost,which i s about twenty cents per f i l t e r . The f i l t e r holder was made from a 2 inch brass c y l i n d e r .  The up-  per h a l f was l j inches deep and threaded t i g h t l y into the 3§ inch bottom section.  A 1/8 inch r i n g to support the f i l t e r was dsoldered  to the inside  of the bottom section so that as t h e top and bottom were screwed the f i l t e r was clamped into place.  to-gether  The ester used to produce the aerosol  was p r a c t i c a l grade di-n-octylphthalate purchased from the Eastman Chemical Company. The experimental set-up was similar*- when the venturi nozzles were being tested except that the 2 inch reducer coupling holding  the screen was  replaced by a rubber stopper to hold the venturi tube. The original/.' v e n t u r i , A, was designed by Forrest (2).  Figure 2  i s a f u l l scale diagram of this venturi nozzle s e t i n the rubber stopper. Two other ventaris B and C were designed s i m i l a r ^ to the f i r s t . v e n t u r i , D, was designed as two pieces.  A fourth  One piece was a 13 mm. glass tube  necked down t o 8mm. and then belled outwards.  This piece was supported by  a rod through the rubber stopper with which the tube could be raised or lowered r e l a t i v e  t p the bottom piece, which was a piece of tubing  through the stopper.  passing  A u.8 cm. diameter by 0.38 cm. t h i c k p l e x i g l a s s cap  could be attached to the upper piece to serve as an impingement p l a t e . The dimensions of the various venturi's are tabulated on the next page  e  Venturi  Throat Diameter  Port Diameter  A  5.69  2.87  B  3.91  2.6k  C  7.00  2.61;  D  7.93  open  PROCEDURE; The percaent transmittancy data required f o r the quantitative analys i s of esters was obtained using a Coleman spectrophotometer i n the Chemistry Department of the U n i v e r s i t y of B r i t i s h Columbia.  An a n a l y t i c a l determina-  t i o n was made on 10 ml. of pure petroleum ether (30 - 60° C) and a s i m i l i a r run was made on 10 ml. of petroleum ether containing some di-n —octyphthalate and the l i g h t transmission measurements at various wave lengths of both these solutions were obtained. To obtain the c a l i b r a t i o n curve a single drop of the ester was weighed out i n a 100.,.mTL» volumetric f l a s k .  The f l a s k was then f i l l e d up to  the 100 m. mark with d i s t i l l e d petroleum ether.  To obtain a point on the  c a l i b r a t i o n curve a volume of t h i s stock s o l u t i o n was pipetted into a 250 ml. wide-mouthed eriewieyer f l a s k and then d i l u t e d to 10 ml.  Then 0.3 ml.  of 2.5 weight percent sodium hydroxide and 0.3 ml. of 2.5 weight percent hydroxyilamine hydrochloride were added t o the ester s o l u t i o n i n the e r l e n — meyer.  The petroleum ether was then evaporated i n a water bath  maintained  at 67° C. inarperiod of 12 minutes, a f t e r which the f l a s k was placed i n another bath and cooled at 25° C. f o r 1 minute.  Ten ml. of d i l u t e modified  solution A was pipetted i n t o the f l a s k over a period of 3/k minutes. The solution was swirled f o r \ minutes and them poured into a curvette and a balance was made dn the K l e t t - Summers on meter within \ minutes.  This  procedure was repeated f o r various weights of ester up to about one milligram.  T  o ^^BBJEJJ/^ •  ^STOPPER ^  FIGURE  DEPT. OF  CHEMICAL  U. B.  C.  ENG.  2  VENTURI  NOZZLE A  D. A.  OUTHRIE  FULL  SIZE p  14-  , The zero point f o r the K l e t t - Summerson meter was 95% ethanol. ;  The analysis f o r the mist samples was s i m i l a r e x c e p t that the m i l l i p o r e f i l t e r was treated with 10 ml, of petroleum ether f o r 5 minutes. Moreover i t was at times necessary to remove any s i l i c a gel that had been carried over onto the f i l t e r .  This was done by f i l t e r i n g the ether s o l u t i o n  a f t e r the 5 minute extraction period through a lw2f> cm. paper f i l t e r .  The  f i l t e r paper was then washed with 2 ml. of petroleum ether and then the analysis was carried out as f o r the c a l i b r a t i o n curve. Before any work could be done with the generator, i t was to  calibrate a l l the flowmeters•  metered through a wet-test meter.  necessary  These were calibrated using clean, dry a i r The volume of a i r metered, i t s pressure,  and i t s temperature were a l l recorded as also was the absolute pressure on the i n l e t side of t h e c o r i f i c e . A f t e r heating the vaporizer bath to 132° to 162°  C. and the reheater bath  C., 25 ml. of fresh di-n-octylphthalate were placed i n the vaporization  chamber and the nichrome c o i l , which had been p r e v i o u s l y coated with four layers of a saturated s o l u t i o n of sodium chloride, was f i x e d into p o s i t i o n . The a i r flow was adjusted to pass the desired volumes into the rniucleation and vaporization chambers.  The nichrome c o i l was  then connected  stant voltage transformer and the current was adjusted to 2.67  to the con-  amperes.  A f t e r the generator had been operating f o r an hour three microscope s l i d e s were coated wi th/^aqueous s o l u t i o n of gum a r a b i c .  This was done by  putting a s ingle drop of s o l u t i o n on to a s l i d e and then s preading i t with another s l i d e .  Using this method the formation of bubbles can be avoided.  After the glue had become tacky, the aerosol was allowed to j e t into the s l i d e through a 6 mm,  glass tubing.  No cover s l i p was used; instead the  s l i d e s were placed i n a calcium chloride d i s s i c a t o r and allowed to dry f o r about two hours.  At the end of t h i s period the droplet diameter  was  15" measured using the micro-hardness t e s t e r attachment f o r the Zeiss microscope i n the M e t a l l u r g i c a l Department of the University of B r i t i s h  Columbia.  A f t e r a suitable homo;g3nous aerosol had been produced the gas stream was sampled by metering the gas througha^millipore f i l t e r .  The amount of  ester deposited on t h i s f i l t e r was determined using the a n a l y t i c a l method outlined. erage  This  measurement was made several times during a run and the av-  was used as the i n l e t concentration. The gas stream was then passed through the 2\ inch column contain-  ing  the s i l i c a g e l and the aerosol concentration i n the e f f l u e n t stream was  measured.  The s u p e r f i c i a l gas v e l o c i t y through the bed was v a r i e d by bleed -  ing  - o f f some of the flow from the generator or by d i l u t i n g the flow with clean  dry  air.  The mist concentration i n the e f f l u e n t gas stream was measured at  each v e l o c i t y .  This procedure was repeated f o r two bed weights.  of aerosol removed by the empty column was also determined.  The amount  The e f f e c t of  i n l e t concentration was also studied. The venturi nozzles were tested i n a similrar- fashion and the weight of s i l i c a g e l entrained i n the gas stream was measured a t several velocities. The beds were sampled p e r i o d i c a l l y .  The s i l i c a g e l l removed was  mixed with petroleum ether, the r e s u l t i n g s o l u t i o n was f i l t e r e d and the f i l t r a t e was analysed f o r ester content.  \6  RESULTS? I  ANALYTICAL PROCEDURES. Table 1.  Percent transmission of hydroxamate s o l u t i o n versus wave length i n microwavelengths. YJave length  % transndttancy  Table 2 .  350  100  375  80  liOO  66.6  U5o  62.5  5oo  ;5?a  550  61.8  600  68.5  625  73.2  650  78.U  675  81.U  700  81.7  Times found most suitable f o r a n a l y t i c a l steps. Step  Time - minutes  Evaporation -at 67°  12.0  at 25°  1.0  Cooling  Addition of s o l u t i o n A  @.75  Swirling .  0.50  Balancing of meter  0.25  Extraction of f i l t e r  5  These data are plotted i n F i g s . 3, and show c l e a r l y a maximum adtsorption i n the range of 500 mic.  ^he timed procedure given i n Table 2 was  found to allow accurate and reproducible analyses.  \7  90  )  30  c  70 )  \  c  60  [60  40  400  300  500 WAVE  FIGURE  3  LENGTH  600  700  mX  TRANSMITTANCY VS. WAVE HYDROXAMATE IN 95 %  LENGTH OF ETHANOL  FERRIC  Table 3.  C a l i b r a t i o n data f o r the Klett-Summerson meter f o r di-ni-octylphthalate, mgm.  di-n*-octylphthalate  Klett-Summerson Rdg.  0  8  0.1368  U$  o.nih  59  0.3U20  102  O.lilpU  115  0.5130  135  0.681 0  195  t  These r e s u l t s are shown on graph k»  Since the K.S. reading i s actu-  a l l y the logarithm of one minus the transmittancy value, the equation of the l i n e can be written, S » 261.8C +• 9.6 which i s log ( 1-1  ) = 261.8C+ 9.6  or which again i s 26l.8c I - I • c T  T  r  0  which i s a form of ^eer's Law. where  /  S = Klett-Summerson reading C = weight of ester - milligrams I B i n t e n s i t y of transmitted l i g h t Im Q  i n t e n s i t y of incident l i g h t  e - exponential e  A l l straigt lines are f i t t e d by method of least squares except where otherwise stated.  FIGURE 4  CONCENTRATION FOR  VS  K. S.  Dl- OCTYLPHTHALATE  READING  Table i i .  Rate of color fading of various hydroxamate s o l u t i o n s . Time elapsed  Klett-Summerson  sees.  Meter Reading  mgm. P.O.P.  Number 1  25  117  .101  5o  115  .to  90  112  .391  120  107  .372  20  68  .223  kO  67  .219  60  67  .219  120  62  .208  30  120  .1*22  60  118  ,!o5  90 120 300  118  ,1O5  Number 2  Number 3  1300  116 111;  .1*07 .UOO  110  .381;  These valves are shown plotted i n F i g . 5> and indicate that i f readings can be taken within  15  seconds, the error i n the naalysis due to a  few seconds variation either way w i l l not be large.  I t i s also apparent  that  the color fades steadily and there is no "preferred" time at which readings should be taken.  22. Table 5.  C a l i b r a t i o n Curves f o r Various Aromatic E s t e r s .  mgms. dioctylphthalate  Cenco meter mgms, rdg. ' n^butylphthalate  Cenco meter rdg.  mgms. Cenco meter e t h y l benrdg. zoate  O.Ou98  87.O  0.0969  57.0  0.294O  38.0  0.1328  76.0  0.1610  55.5  o.mao  29.5  0.3320  57.0  0.3230  1*5.0  0.5880  2U.0  0.4980  46.O  0.1.850  35.0  0.8820  16.0  0.5976  52.0  O.646O  27.0  0.6972  3U.5  0.9690  •18.0  0.7968  28.0  O.8964  25.0  0.9960  22.5 The equation f o r the various l i n e s of f i g u r e 6 are;  1.  f o r di-n-octylphthalate  _  -0.625c  T  I « I e c  2.  f o r n-butylphthalate I - 1  3.  e  -0.600C  f o r ethyl benzoate I - I  c  e --  6 1 2 C  Table 6. E f f e c t of Parent A i d . c  Mg. of E t h y l Benzoate  mg. o f Benzoic Acid  Cenco Meter M s . _____________  0.29U0  0  48.O  0.2940  0.1730  58.0  0.29UO  0.1730  59.0  0.2940  0.3u50  70.0  0.2940  0.3U50  68.0  The data g i v e n i n Table 5 a r e > p l o t t e S - i n F i g . 6 and show that t h e complex formed obeys Beer's Law s a t i s f a c t o r i l y f o r a v a r i e t y of e s t e r s over t h e range of c o n c e n t r a t i o n s i n v e s t i g a t e d .  0.1  0.2  0.3  0.4  0.3  0.6  MILLIGRAMS  FIGURE  6  0.7 OF  0.8  0.9  I.I  1.2  ESTER  CONCENTRATION  VS.  READING  THREE  FOR  1.0  CENCO  METER  ESTERS  a4  II.  Generator Operating Conditions.  Vapourizer Temperature  s 132° C.  Reheater temperature  - 162° C.  ^'Njucleation c o i l current  z°2.67 amperes  Air flow to preheater  - 9.88 liters/min.  Air flow to vnucleation r 8.78 liters/min.  chamber  Air flows referred to 1 atmosphere and 70° F« A l l velocities reported are superficial velocities. For the fluidized bed and for venturi D, the velocity was calculated on the basis of the 2.25 inch column. For  Venturis  A, B, and C, the velocities were calculated  on the basis of the various throat diameters l i s t e d . It has been found more convenient to w ork with P a 100 - E where E is the collection efficiency expressed as a percent; P then i s percent not removed. The bed was 150/200 Tyler mesh s i l i c a gel. III. Table 7.  Mist Removal i n the Fluidized Bed and i n the Venturi Nozzles. Effect of inlet concentration on collection efficiency.  weight 651 gms. = 25.35 gms* per sq. cm^  Bed  Bed height at rest 5 k2 cm.  Run  Velocity  Inlet Concentration  P %  No.  cm./sec.  mgms./ft.3 Co.  Not removed  8E  11.88  .690  22.2  9E  11.07  ,70k  25.2  6E  11.25  .728  28.6  5E  10.U8  .782  2U.6  2JE  11.82  .877  22.8  50 CO  <  540e x  o  <30  a  Ul  •o  • o -  AC  -C)  ©20  in 1 0 o  K kl  0.  0.6 8  .70  .72  .74  INLET  FIGURE  7  EFFECT  OF BED  i  •76  ESTER  INLET  •78  .82  .80  CONCENTRATION  C0NC. ON  WEIGHT  84  "FILTERED"  MIST  REMOVAL  35.3 5 GMS/SQ. CM.  86  .90  MGMS / C U F T  792  Table 8 .  E f f i c i e n c y measurements i n empty column. Velocity cm./sec.  Table 9.  % not removed  3.U1  72.3  6.90  70.1  11.82  82.6  Results f o r the 3 4 I gm. a 1 3 . 2 5 gms. per sq. cm. f l u i d i z e d bed.  Bed depth at rest - 23 cms. Run No.  Vel. cm./sec.  1 v/Vei;  P % not removed  P % not r e moved- corre cted  Condition of Bed  12A  3.08  0.568  13.6  19.U  -bed depth 25 cms.  5B  1.05  O.U97  16.6  23.3  -not quite f l u i d i z e d  8B  5.71  O.4I8  m.i  19.4  -particles  11A  5.72  6.L.18  12.0  16.5  10A  6.79  0.383  16.0  21.7  o.369  15.7  ,21.1  7B  7.32  9A  8.75  0.338  19.5  26.3  6B  10.32  0.311  19.4  24.7  8A  11.82  0.291  22.5  28.3  i  bouncing  on upper bounds^' of bed. -bed depth 28 cms.  -bed well f l u i d i z e d  11.82  0.291  2li.8  31.2  UB  11.8.2  0.291  21.3  26.8  LIB  11.85  0.290  19.1  2U.1  lliA  lj.,10  0.277  25.6  31.5  12B  13.51  0.273  21.2  26.1  13A  14.35  0.26U  29.1  35.0  of g e l , excessive  9B  LU.lt8  0.263  28.6  3lu8  jetting - d i f f i c u l t to measure depth.  15A  -no j e t t i n g or slugging. -heavy carry over  30  u  28 o  < 26  5 2 4 <  j  ^ \  kl  te CO 2 2  2  i  o20 •  kl  0.  18 o  16 5 6 SUPERFICIAL  FIGURE  8  EFFECT  OF  7 GA8  VELOCITY  8 VELOCITY  ON  MIST  9  10  II  12  FOR  EMPTY  13  CMS/8EC.  REMOVAL  COLUMN  34  Figure 9 i s a plot of superficial gas velocity, Vo, against the percent not removed, PJ both corrected and uncorrected values of P are Figure 10 i s a plot of l /  plotted. Table 10.  V  Q  versus the percent not removed.  Results for the 651 gms - 25.35 gms. per sq. cm. fluidized bed.  Bed height at rest - kk cms. Run No f  Vel. cm./sec.  ,1 /"Vo.  . P % not Eemoved  P % not removed-corrected  Condition of bed  8C  3.20  0.558  11.2  16.0  7D  k.kB  O.U72  15.0  21.1  7C  1+.78  O.U57  11.2  15.6  6C  5.85  0.I4IU  12.0  16.1,  -depth = kk cms.  5C  7.82  0.357  18.8  25.0  -well fluidized  8D  7.87  0.356  19.5  25.9  5E  10.1+8  0.309  2U.6  31.6  9E  11.07  0.301  25.2  32.1  6E  11.25  0.299  28.6  36.3  IjE  11.82  0.291  22.8  28.7  UD  11.82  0.291  22.5  28.3  13C  11.82  0.291  21.1  26.6  9C  11.82  0.291  17.8  22.U  10E  11.82  0.291  18.8  23.7  8E  11.88  0.290  22.2  27.9  5D  12.55  0.283  20.2  25.2  6D  12.55  0.233  2U.8  30.9  10C  12.90  0.279  17.8  22.1  -jetting  11C  13.05  0.277  19.6  2U.3  -bed depth 51* cms. „  12C  13.20  0.275  18.0  23.2  -not well fluidized  -depth r 52 cms.  o  x  6  o  X  o  X o  -Oo  o  o  KEY CORRECTED  -Q-  X  UNCORRECTED  C  o  6 SuPERMCIAL  EFFECT  7 G A 8  OF VELOCITY  8 VELOCITY  ON MIST  9  10  I I  12  13  14  C M / 8 EC'  REMOVAL.' BED WT. 2 5 . 3 5 GMS/SQ CM.  34  <  O  ,26  (  < Z  22 <0  c 18  O  )u  u o cc Ul  °- 14  o  o  10  6.0 I V/SUPERFICIAL  FIGURE 12  EFFECT  OF VELOCITY  GAS  VELOCITY  ON MIST  CMS/SEC.  REMOVAL. BED WEIGHT 25.35 GM>5Q. CM. N  34  (0  <  KEY  30 X  ©  o  BED  *  25.33 0M8/8Q. CM.  BED — < > —  OVERALL  o  26  13.25 0M8/8Q. CM.  X  (  z z  < £22  X  CO  o  2  (  O-  18 ui o  X  X X  OC Ul  °- 14  X  .  o  X  o  10. 2.0  2.4  2.8  3.2  3.6  4-4  40  4.8  5.2  5.6  6-0  I v/SUPERFICIAL  FIGURE 14  EFFECT  OF VELOCITY  OAS  VELOCITY  ON MIST  CMS/SEC.  REMOVAL FOR  FLUIDIZED  BEDS  Figures 11 and 12 are plots of the data on the preceding page only and figures 13 and Ik show the r e s u l t s f o r both f l u i d i z e d beds. Table 11,  Results f o r venturi A, Throat area -  Table 12.  Port area  r  Bed weight  =  2  5 . 4 4 sq. ram.  .9h  sq. mm.  12  iQO grams.  Run No.  Velocity cm./sec.  P % not removed  6F  1195  61.9  7F  1195  60.U  Results f o r venturi B Throat area Port area Bed weight  s  12.01  sq. mm.  10.92 sq. mm. r 100 grams. Velocity cm./sec.  Run No.  P % not removed  888  64.2:  888  58.8  7P  1150  60.5  6P  1150  60.9  9P  1750  59.7  10P  1750  65.5  UP  2570  6U.9  12P  2570  58.8  17P  2570  59.6  18P  2570  61.0  13P  2810  5U.2  luF  2810  55.7  15P  3210  62.7  16P  3210  65.9  5P 6P  !  66  o  O  o  o  CO  < 60  VENTURr A  o  (J  /-^  *v/  CJ  !  o  ii fI  65  (J  u OC \  z Z  Ul  o cc  Ul  43 tt -  o. 40  800  1000  12 O O  1 4 0 0  1600  8UPERMCIAL  FIGURE 15  EFFECT  OF  It1 0 O GA8  2000  212 0 0  VELOCITY  VELOCITY  ON  2400  2600  2800  9 0 0 0  3200  CM8/8EC  MIST  REMOVAL '.  VENTURI  B  t 0*  31  Table 13. Results for venturi. C. Throat area  s  3 8 . ^ 0 sq. mm.  Port area  r  10.92 sq. mm.  Bed weight  - 100 grams.  Run No.  Velocity cm./sec.  P % not removed  19N  299  63.7  20N  299  57.9  17N  379  62.3  18N  379  61+.9  15N  380  65.8  16N  390  67.8  7N  514  59A7  8 N  514  61.2  5N  80a  6u.l  6N  80lt  55.6  13N  801+  60.5  lilN  80 k  63.2  9N  923  65.0  ION  923  59.2  11N  985  5U.2  12N  985  54.2  Graph 17 i s a plot of the data for venturi's B and increase  showing t h e  i n removal e f f i c i e n c i e s observed >;ith i n c r e a s i n g v e l o c i t i e s .  plot of t h e o r e t i c a l  A  t a r g e t e f f i c i e n c i e s f o r the s o l i d and a e r o s o l p a r t i c l e s  used  and based on the' v a l u e s o f Langmuir and. Bjod'gett (9), i s a l s o s h o r n f o r c o m p a r i son on t h e same graph.  FIGURE  16  EFFECT  OF  VELOCITY  ON MIST  REMOVAL ! VENTURI  C  to 00  FIGURE 17  EFFECT  OF  VELOCITY  ON  MIST  REMOVAL ! VENTURIS  BSC  Table l U .  Results f o r Venturi D, with no cap. Throat area Open port gap Bed weight  =  U9.32 sq. mm. =  l.£9 cms.  100 gms.  Run  Velocity  P % not  No.  cm./sec.  removed  9J  I1.48  62.2  10J  U.U8  64.O  5K  6.29  71.6  6K  6.29  68.3  7J  6.48  65.4  8J  6.48  60.6  9K  8.16  75.7  10K  8.16  70.5  5J  8.27  72.4  6j  8.27  79.7  11J  12.0a  68.8  12J  12.0U  73.2  7K  12.04  73.5  8K  12.Oil  67.1  13J  13.00  80.3  I4J  13.00  78.9  5K  14.81  90.5  6K  1U.81  85.9  41 Table 15.  Results f o r Venturi D with p l e x i g l a s s cap. Bed weight = 100 Open port Run No.  gms.  gap - 1.59  P £ not removed  Velocity cm./sec.  5.59  10L  76.0  ILL  5.59  81.2  8L  8.23  79.2  9L  8.23  81.5  8M  12 .Oli  72.9  5L  12.  Ok  70.6  UL  12.0k  70.9  lk.55  94.8  7L  14.55  74.6  4M  L U . 8®  78.2  5M  14.80  74.5  6M  14.80  65.8  6L  The results tabulated Table 1$.  cms.  i n Tables lk and 15 are plotted on f i g u r e 1 8 .  Solids flow f o r venturi B. Velocity cms./sec.  Wt. of gel collected gms. per min<>  723  2.0  1151  2.9  1418  8.6  1490  12.2  2110  17.8  2285  14.8  2880  15.3  100 0  600  1200  1400  SUPERFICIAL  FIGURE  19  EFFECT  OF  1600  1800  OAS  VELOCITY  VELOCITY  ON  2000  2200  2400  2600  2800  CM8./SEC.  SOLIDS  FLOW  VENTURI  B  3000  Table 17.  Solids flow results f o r venturi C, Velocity cms./sec.  Wt. of gel collected gms, per min.  275  3.0  455  3.8  588  4.7  719  5.8  902  11.0  i results f o r venturi D, Velocity cms./sec.  ¥t. of gel collected gms. per min.  2.89  4.3  5.91  19.4  6.15  22.3  8.67  23.1  11.82  25.2  11.88  24.6  H.72  22.U  10  1000  SUPERFICIAL  FIGURE  20  EFFECT  OF  6AS  VELOCITY  VELOCITY  ON  1100  CMS./SEC.  SOLIDS  FLOW! VENTURI  C  1200  4<>  4*t  LY.  Results of Smoke Measurements* Average di-n-octylphthalate droplet diameter - 0.869 miserons.  Table 19.  D i s t r i b u t i o n data f o r aerosol measurements. Droplet Diameter Range  No. of droplets i n range  Cumulative %  Q)*50 or less  3  1.36  0.50 - 0.55  2  2.27  0.55 - 0.60  5  4.53  0.60 - 0.65  4  6.34  0.65 - 0.70  12  11.76  0.70 - 0.75  23  22.16  0.75 - 0.80  37  38.90  0.80 - 0.85  43  58.3U  0.85 - 0.90  22  68.38  0.90 - 0.95  41  86.91  0.95 - 1.00  14  93.23  1.00 - 1.05  6  95.93  1.05 -  1.10  3  97.29  1.10 -  1.15  1  97.74  - upwards  5  100.00  1.15  Figure 22 i s a plot of the above r e s u l t s .  0.5S  .60  . 65  .70 AEROSOL  FIGURE 22  AEROSOL  .75  . 80 DROPLET  DROPLET  . 85  .90  DIAMETER  DIAMETER  .96  1.00  MICRONS  DISTRIBUTION  1-0 6  110  1.15  DISCUSSION; The curve shown i n f i g u r e 3> the p l o t of transmittancy versus wave length, agrees f a i r l y well with those obtained by H i l l (li) and Thompson (17). Since a minumum occurs i n the 5(XW(^ region a 520  f i l t e r was used i n the  Klett - Summerson meter. H i l l (U) reported that the hydroxamate s o l u t i o n obeys Beer's Law up to concentration ofaimilligram of ester f o r f a t t y a l i p t h a t i c compounds. This means that, since Beer's Law i s of form I : I where  D  C ~  k c  I - transmitted l i g h t i n t e n s i t y I «» incident l i g h t i n t e n s i t y Q  c z  concentration  k ; extinction coefficient a p l o t of l o g ( ~Y~ \ against the concentration should be a s t r a i g h t l i n e , o / As the scale on the Klett-Summerson meter was logarithmic a p l o t of K, S. reading against concentration yielded a s t r a i g h t l i n e .  The c a l i b r a t i o n curve  shown on f i g u r e h agrees very well with previous curves, proving that r e producible r e s u l t s can be obtained using the timed method described i n the procedure s e c t i o n . The several equations f o r the curve of figure h were l i s t e d t o show the  r e l a t i o n s h i p between the meter reading and the concentration of ester©  The f i r s t  equation i s the one used i n c a l c u l a t i n g , whereas the second and  t h i r d equations are written t o show that the hydroxamate s o l u t i o n obeys Beer's Law. I t was noticed that the color of the hydroxamate s o l u t i o n faded with time, p a r t i c u l a r l y i f there was any l i q u i d petroleum ether remaining i n the easTenme^r f l a s k .  Figure 5 shows the rate of fading f o r various  concentrations  of di-n-octylphthalate.  I t should be noted that the i n i t i a l rate of fading  i s more rapid than the rate a f t e r a minute or so.  The data f o r the e f f e c t  of the parent acid and the c a l i b r a t i o n curves of figure 6 were obtained working  i n conjunction with R. Rye (15).  Rye used the exact method as proposed  by H i l l (u), namely to evaporate the . dther solution to dryness and then f o r 5> seconds longer; however the r e p r o d u c i b i l i t y of t h i s method was very dependent i n the s k i l l of the analyst. The parent acid a f f e c t s an increase i n the amount of l i g h t /transmitted or rather i n h i b i t s the formation of the red-colored complex. The idea i n doing the work on the other esters was  to determine  if  the color was formed by the acid part of the ester alone; t h i s would mean that the n-butylphthalate and the di-octylphthalate should have had the same c a l i b r a t i o n curves.  From the results i t was decided that the rest of the  compound affected the color formation. Since the curves of figure 6 are not used elsewhere i n the report the "best" l i n e i s f i t t e d by eye. Before any work could be done on determining removal e f f i c i e n c y , i t was  necessary to f i n d the operating conditions required f o r producing a  homogenous aerosol.  I t should be noted that the operating conditions decided  upon are considerably, d i f f e r e n t from those suggested by LaMer ( 6 ) . However i t seems that one difference must have balanced another because a reasonably homogenous aerosol  was produced.  The aerosol droplet s i z e was measured using  the L e i t z microscope i n the M e t a l l u r g i c a l Department of the University of B r i t i s h Columbia.  The mist sample was c o l l e c t e d by l e t t i n g i t impinge onto  a glass s l i d e coated with gum arabic s o l u t i o n . to determine just how tacky  Although some e f f o r t was made  the gum arabic should be i n order that the drop-  l e t s adhere to i t , no d e f i n i t e conclusions were reached.  I t i s suggested  that the several s l i d e s be coated with the glue and l e f t f o r various lengths  of time from 2 to  £ minutes.  In t h i s way some, i f not a l l , of the s l i d e s  w i l l be s u i t a b l e - % e n making the a c t u a l measurement of the droplet s i z e , i t was found that i t was very advantageous to measure a single c l u s t e r of droplets.  This meant that the microscope d i d not have to be  refoeused.  Figure 22 shows the droplet s i z e d i s t r i b u t i o n f o r the di-n-octylphthal a t e mist. Considerable d i f f i c u l t y was found i n getting the generator to produce a constant mass loading.  I t was thought that perhaps the m i l l i p o r e f i l t e r  was not stopping a l l the droplets.  This was disproved by using two  i n series and measuring the amount of ester collected on the second.  filters In  a l l cases t h i s amount was so s l i g h t that i t can be considered n e g l i b l e . Improvement i n steadying the generator mass loading was  achieved  by shortening the depth of the sampler, by p l a c i n g some glass wool i n the l i n e between the reheater and vaporizer to remove entrained.droplets, and by always coating the c o i l with the same amount of solium c h l o r i d e . these a l t e r a t i o n s , the mist concentration produced by the generator constant a f t e r steady state conditions were reached.  With was  This usually required  at l e a s t one hour. Several tests were made to determine whether or not the m i l l i p o r e f i l t e r was however,  soluble i n the petroleum ether.  /^wlre  I t was found that they- were notj  thought to be s t r u c t u r a l l y deformed.  The amount of e s t e r l e f t on the paper f i l e r was  about 10$ and so  i t was necessary to adjust the i n l e t concentration when reporting the range of i n l e t concentration studied. The results obtained on the f l u i d i z e d beds contradict those by Meissner and Mickley (10).  obtained  Whereas the r e s u l t s of this work show that the  removal efficiency/- decreases as v e l o c i t y increases, the r e s u l t s of Meissner and Mickley (10) show? that the c o l l e c t i o n e f f i c i e n c y increases as v e l o c i t y  sz  increases.  I t i s proposed that of the two  mechanisms, i n e r t i a l and d i f f u s i o n a l ,  that the more dominant one i s d i f f u s i o n a l . The target e f f i c i e n c y to be expected i n this system of a d i l u t e mist i n a f l u i d i z e d bed can be estimated from the results given by Langmuir and Blodgett (9),  The numberical values obtained probably have a f a i r degree of  uncertainty;.}; but the order of magnitude should be an i n d i c a t i o n of the r e moval mechanism operating i n these t e s t s . The dime.nsionaless group  U  t  Vo  has been evaluated(see calculations  section) f o r t h i s system and i t i s obvious that f o r v e l o c i t i e s over the range of 1 to 15 cms. per second that the target e f f i c i e n c i e s are, f o r a l l p r a c t i c a l purposes, zero over the entire range,, Using the equation f o r d i f f u s i o n a l displacement given e a r l i e r , the average l i n e a r displacement of a p a r t i c l e of average diameter of 0,87 microns i s about 10.7 microns i n 2.85 seconds.  This may be compared to the average  bed p a r t i c l e size of 90 microns and a bed void f r a c t i o n of 0.i;3.  I t i s shown  i n the calculations that every aerosol p a r t i c l e must t r a v e l 7,9 microns, which means c o l l e c t i o n e f f i c i e n c y should be about 130$.  This i s not v a l i d , of course,  to a high degree of accuracy because the void space i s not spheroidal as was assumed, and hence the average distance each droplet must t r a v e l w i l l be greater since a sphere represents the minimum dimensions f o r a given volume. The order of magnitude i s i n t e r e s t i n g since i t indicates the importance of the d i f f u s i o n mechanism and i t would appear that there are sound reasons f o r assuming that the c o l l e c t i n g action of a f l u i d i z e d bed f o r the conditions used here i s almost e n t i r e l y by d i f f u s i o n .  The d i f f u s i o n equations  indicate that the d i f f u s i o n a l displacement i s proportional to the square root of the time and therefore to.  1  •  The data was plotted t h i s way on  figures 10, 12, and l i t , and results^ while no better than those depicted by figures 9, 11, and 13j are c e r t a i n l y no worse.  The assumption here i s that  the l i n e a r movement accomplished by d i f f u s i o n i s d i r e c t l y proportional to the c o l l e c t i o n e f f i c i e n c y .  Some ; terror i s introduced i n this graph by the  f a c t that the time i s not quite proportional to the s u p e r f i c i a l v e l o c i t y due l a r g e l y to the varying bed expansion and therefore to bed void volume; however i t was not worth correcting f o r the varying void volume because of the  spread  of the data. The reason why Meissner's and Mickley s 1  (10) results d i f f e r from  these i s that the droplet s i z e range used by them was whereas the average mist s i z e used here  was  0.87  from 2 to 10 microns,  microns.  Moreover the  concentrationand v e l o c i t i e s used by Miessner and Mickley were both greater than those used i n this work. That the removal e f f i c i e n c y of the empty column decreased with an increase i s v e l o c i t y i s thought to have been caused i n part by the blowing over.. at'-'higher v e l o c i t i e s , of some aerosol droplets which might have adhered to the walls at lower v e l o c i t i e s .  This e f f e c t of v e l o c i t y on mist removal  f o r the empty column could also be attributed  to d i f f u s i o n a l mechanisms.  Figure 7 v e r i f i e s that i n l e t concentration has no e f f e c t on c o l l e c t i o n e f f i c i e n c y over the range studied.  This agrees with r e s u l t s reported by  Meissner and Mickley (10); however no s i g n i f i c a n t change i n c o l l e c t i o n e f f i c i e n c y by was  obtained/increasing the bed weight.  I t i s quite possible that the mist was  This f a c t i s shown by figure  13.  -so d i l u t e that i t was not possible  to detect any improvement of the heavier bed over the l i g h t e r bed.  Meissner  and Mickley (10) reported that an increase of bed weight improved the c o l l e c t i o n e f f i c i e n c y , but they worked with a more concentrated  mist.  An attempt to obtain greater impingement e f f i c i e n c y was c a r r i e d out using venturi contactors, i n which f i n e s i l i c a gel entered at throat p o r t s .  At the moment of contact between the f l u i d and the solids i n the venturi throat relative velocites were high-up to 3000 cm./sec. From the values given for target efficiency the following theoretical results can be predicted: Vo  U  Vo  t  He  500  O.lu  0.13  1000  0.28  0.28  2000  0.56  o.n  3900  0.81*  0.57  Up to 57$ collection efficiency based on an isolated target sphere and the space i t sweeps night be expected. This is a reasonably true picture 7  since, roughly there were about 10'' collecting spheres per minuter passing through the apparatus compared to 10^" rosol particles per minute. 0  ae  Collection  by diffusion mechanisms might be expected to be at a minimum because of the relatively large separation of the collecting particles i n the venturi and the extremely short collecting time. Percent removed i n the venturi using tube B as an example, varies from 37$ at l,000cms. per second to l\2% at 3,000 cms per second. The results obtained are of the expected order of #  magnitude, although the dependency of the efficiency on velocity i s considerably less than was expected. Figure 17 shows the actual and the theoretical results• Figures l5> 16, 17, and 18 are plots of velocity versus percent not removed for the various venturi nozzles used. Although the removal efficiencies obtained are not too good, they do improve with increased velocities, indicating that impingement i s actually the collecting mechanism. The results shown by figure 18, for venturiD can be explained by the fact that the amount of air jetting up through the bed seemed greater for the uncapped nozzle than for the capped nozzle.  Because of this the former would simply be a poorly  fluidized bed and would be expected to behave as i t d i d .  I t should, however,  be emphasized that the results for venturi D are not too useful since i t was impossible to determine throat velocities because only some of the gas passed up through the venturi. The graphs of the solids flow versus v e l ocity, figures 19, 20 and 21, were determined to show how l i t t l e solids was picked up by the gas stream and to enable one to calculate the number of particles passing through the throat per minute. A sirniliar curve f o r venturi A can be found i n the report by Forrest ( 2 ) .  SUMMARY: The colorimetric analysis as reported was quite satisfactory and i t was used to measure as l i t t l e as 0.1 mgms. of di-n-octylphthalate. I t was found that the La^er-Sinclair generator, under suitable conditioi produced a reasonably homogenous aerosol of average droplet size 0.869 microns. The ester used was di-n-octylpmthalate. The results reported for the f l u i d i z e d beds of 150/200 mesh s i l i c a gel show that the removal efficiency was independent of the i n l e t concentration over the range 0.765 to 0.965 mgms. of ester per cubic foot of a i r .  They also  show that the efficiencies were not affected by increasing the bed weight from 13.25 to 25.35 gros* per sq. cm. Theoretical calculations have been included to show the importance of the diffusional forces compared to i n e r t i a l forces as affecting this mist removal.  The maximum removal efficiency'obtained was  88.8$ at a v e l o c i t y of 3.20 cms. per second and a bed weight of 13.25 gms. per sq. cm. In order to increase the relative velocities of the aerosol droplets to the s i l i c a gel particles to study impingement mechanisms, venturi contactors were used.  Although i n these cases the removal efficiencies were  low - 35$ to U5$ - they did increase with an increase i n v e l o c i t y indicating that the removal was, i n fact, caused by impingement mechanisms.  I t has been  shown that the amount of s i l i c a g e l entrained i n the gas stream was r e l a t i v e l y small however^this f a c t i s not too important because t h e o r e t i c a l calculations have shown that expected e f f i c i e n c i e s would The  be about  even f o r much greater s o l i d s flow.  actual e f f i c i e n c i e s obtained are o f the correct magnitude as predicted by  the t h e o r e t i c a l c a l c u l a t i o n s j however^the e f f i c i e n c y i s not as dependent on v e l o c i t y as was expected.  J"7  N O M E N C L A T U R E  C  0  =  i n l e t concentration of ester  C  1  =  i n l e t concentration of acid  Cg  =  exit concentration of acid  D^  =  average diameter of s i l i c a p a r t i c l e  Dp  =  average diameter of aerosol droplet  E  =  percent removal e f f i c i e n c y  P  =  100 minus percent removal e f f i c i e n c y  =  target e f f i c i e n c y  j^.  =  terminal velocity  V  =  average s u p e r f i c i a l v e l o c i t y  g  =  gravitational  AS  =  average linear displacement  R  =  gas constant  T  =  absolute temperature  t  =  time  =  Cunningham correction  2(  =  f l u i d viscosity  N  =  Avagadro's number  k  =  extinction  W  =  bed weight per unit area  n  =  empirical constant  S  =  K l e t t , Summerson meter reading  0  acceleration  factor to Stoke*s law  coefficient  BIBLIOGRAPHY; 1.  F i e g l e , F.  Laboratory Manual of Spot Tests p. 1 8 6 - 7 . New York, Academic Press (I9u3).  2.  Forrest, D. B., Batchelor of Applied Thesis, Department of Chemical Engineering, University of B r i t i s h Columbia.  3.  Goetz, A., A . j . of Public Health u3(2) 190-9  U.  H i l l , U. T., Ind. E  5.  H i l l , U. T., Ind. Eng. Chem. Anal. Ed. 19 932  6.  LaMer, 7. K., and Gendron, P. R., Chem. i n anada, h  7.  LaMer, V. K., A i r P o l l u t i o n Chap. 7U.  m  n g  (1953).  . Chem. Anal. Ed. 18 317-19 ( I 9 u 6 ) .  (19U7).  c  UU(1952).  McGraw H i l l Book Co., New York (1952). 8 . Lapple, C. E., F l u i d and P a r t i c l e Mechanics, Chapter 1 3 , and LU. University of Delaware, Newark, Delaware (195U). 9.  Langmuir, I . , and Blodgett, K. B., U.S.A.A.F. Tech. Report No. 5Ul8, Feb. 19U6. U.S. Dept. of Commerce, Office of Tech. Services P.B. 27565. 1238-U2 (19U9).  10.  Meissner, H. P., and Mickley, H. S., Ind. E  11.  Perry, J . H., Chemical Engineer's Hand Book, p. 1013, McGraw H i l l Book o .  n g  . Chem. Ul(6)  c  New York (1950). 12.  Pring, R. T., A i r P o l l u t i o n Chap. 35, McGraw H i l l Book Co., New York (1952).  13.  Product Engineering, p. 2lU (July 195U).  lU.  Reiss, H., and LaMer, 7. K., J . Chem. Phys. 1 8 , 1 (1950).  15.  Rye, R.  Department of Chemistry, U n i v e r s i t y of B r i t i s h Columbia, Personal Communication.  16.  S i n c l a i r , D., Handbook on Aerosols, Chap. 6 , United States Atomic Energy Commission, Washington D. C. (1950).  17.  Thompson, A. R., Australian J . S i . Research 3A, 128-135 (1950).  18.  Wilson, B. W., Australian J . Appl. S i .  19.  Wong, J . B., Rantz, W. E., and Johnstone, H. F., J . Appl. Phys. 26 2UU-9 (1955).  c  c  5 U7-57  (1953).  20. Wong, J . B. and Rantz W, E. Ind. Eng. Chem. 6 p.1371 (June 1952).  DATA AND CALCULATIONS: Table A.  For percent transmittancy of hydroxamate s o l u t i o n versus wave length  'Wave length  B  s  _  Table B.  B_  % transmittancy  _  B  s  / B  r  350  2  2  375  2  2.5  80  u'OO  2  3  66.6  h$0  5  8  62.5  500  16  28  57.1  550  29  kl  61.8  600  1*2  61.5  68.5  625  Uh  60  73.2  650  36  1*6  78.1;  675  22  27  8l.ii  700  9  11.0  81.7  100  Data f o r C a l i b r a t i o n Curve f o r D, 0 . P. on the Klett-Summerson meter. KLett-Summerson meter rdg. 8  milligms• di-octylphthalate  0  li5  0.1368  59  0.1710  102  0.31*20  115  O.I1IO4  135  0.5130  19k  O.68I1O  6o  C. Data f o r rate of color fading f o r t y p i c a l hydroxamate solutions. Run 1 Time sees*  Run 2  K. S. rdg.  mgrris.. D.O.P.,  Time sees.  N  a.  25  117  .101  b.  50  115  .403  c.  90  112  .391  d.  270  107  .372  Rune 3  K.S.  mgms. D.O.P.  rdg.  20  Time sees.  K.S.  rdg.  mgms • D.O.P.  68  .223  30  120  .U22  67  .219  60  118  .Ui5  60  67  .219  90'  118  .105  120  120  .208  120  116  .U07  e.  300  11U  .Uoo  f.  1500'  110  .38U  Uo  Sample calculation f o r run l a using the calculated equation f o r the c a l i b r a t i o n curve.  S  =  261.8 C + 9 . 6  C r S - 9.6 261.B Table D.  117 - 9.6  261.8  =  o.Ull mgms.  C a l i b r a t i o n data f o r various esters. mgms. n-butylphthalate  % transmission  mgms. di-n-o ctylpththalate  % transmission  O.OU98  87.0  0.1328  76.0  0.1610  55.5  0.3320  57.0  0.3230  U5.o  O.U980  U6.0  O.U850  35.0  0.5976  52.0  0.6U60  27.0  0.6972 0.7968 0.896U  3U.5 28.0 25.0  0.9690  18.0  0.9960  22.5  mgms. e t h y l benzoate 0.29UO O.UUlO 0.5880 0.8820  %  transmission 38.0 29.5  2U.0 16.0  0.0969  57.0  -6/ Table E.  Effect of parent acid on hydroxamate formation.  mg. of ethyl benzoate  mg. of benzoic acid  Cenco meter rdg.  0.29U0  0  U8.0  0.291*0  0.1730  58.0  0.29l|0  0.1730  59.0  0.29uO  0.3u50  70.0  0.291*0  0.3li50  68.0  Table F.  Operating data. Vapourizer temperature  =  132°  c.  Reheater temperature  =  162°  c.  Ionization c o i l current  s  2.67 amps.  Diameter of column  -  2.25 i n .  Flow through the enucleation chamber. 1.  Flowmeter reading  _  21.0  2.  Inlet pressure  =  17.0  Flow through the a i r preheater. 1.  Flowmeter reading  •  21.0  2.  Inlet pressure  -  16.0.  The flowmeter calibration curves are listed i n the Appendix C on page 80  «  Table G. Run No.  Data f o r removal by empty column*  Through Bed i n l e t pressure p i n Hg. i n Hg  Bleed-off V o l . of i n l e t pressure flowmeter Sample i n Hg. Rdg. i n Hg.  K.S. Rdg.  DTO: ft.3  2T  0.5  0.3  .502  116  .811  3T  0.5  0.3  .700  159  .816  1*T  o.5  0.3  .500  117  .822  —  —  .600  163  .978  —  —  .503  135  .952  —  —  ,5oo  H*o  .996  0.5  0.3  .5oo  113  o.5  0.3  .601  117  o.5  0.5  .502  120  0.5  0.3  .501  111*  i3T  o.5  0.3  .501  116  UlT  o.5  0.3  .502  119  15T  —  —  . .600  170  1.022  —  —  .6oU  177  1.059  o.5  0.3  .5oo  119  o.5  0.3  .503  117  —  —  .5oo  11*8  1.058  —  —  .500  127  .896  3X  o.5  0.3  1.0.Q1  221  .80 7  l*X  o.5  0.3  .5oo  109  .760  o.5  0.3  1.1*0  10.20  .5oi  101*  .723  o.5  0.3  i.l*o  10.20  .502  99  o.5  0.3  3.10  2.80  .1*98  97  0.5  0.3  3.10  2.80  .5oo .500 .5oo  6T 7T 8T 9T  10T LIT 12T  16T 17T 18T IX 2X  5X  6X 7X 8X 9X 10X 11X 12X  o.5 o.5  0.3 0.3  * indicate'^ second f i l t r a t i o n step was carried out. !' indicates inches of carbon t e t r a - c h l o r i d e .  .502 .501  106 137 137  111 116  .790 .681* .81*0  .796 .812 .833  .836 .816  .679 .671 .736 .972 .972 .773  .831*  Method of Calculation For the T. series the average i n l e t mass loading was calculated and then from these, one value of c o l l e c t i o n e f f i c i e n c y was calculated. The  calculations f o r the X series was s i m i l a r except that i t was necessary  to compute the e x i t concentrations at the several v e l o c i t i e s used. average points were p l o t t e d on f i g u r e 8 .  These  THEORETICAL CALCULATIONS 1.  To determine the value of the dimensionaless group -  Ut Vo g Dp  2U.U (10"*) cm/sec ( l l )  Ut  -  8(10" ) ft/sec  g  •  980 cm/sec/sec  Dp  -  89(10~4) cm (average of 150 to 200 mesh aperature)  Vo  -  variable of 1 to 3000 cm/sec  4  . . Table S  Ut Vo g DP -  o.00028Vo  _  Theoretical target efficiencies for 150 to 200 mesh s i l i c a gel:  7? t  Vo cms /sec  Generator output  fraction collected  Ut Vo g Dp  500  0.1U  0.13  1000  0.28  0.28  2000  0.56  0.1+7  3000  0.81+  0.57  -  1 milligram of ester per cubic foot.  Approx. density of di-n-octylphthalate  0.96  «  /. number of aerosol particles per cu. f t . • (0.01)(3) F  2  Ic  3;  ,10  therefore number o f aerosol particles passing through column  •  10^° per minute. A t r i a l calculation to check/o^aer of magnitude of results from the diffusion equations. Using the data for the 25.35 gsis per sqi.cm.bed weight and Vo, the superficial velocity, equal to 7.82 cm/sec  (Run 5c)  Prom figure 12 the amount of mist not removed " 18.6$. Therefore collection efficiency  - 81.1$.  The bed depth * 52 cms, therefore, volume of bed  *  (area)(height)  • 1335 cc. Since the density o f silica gel » 0.85 gm/cc, and the bed weight * 651 gms then ^ , the void fraction, * 0,43. Then the true linear velocity  - V6/0.U3 * 2.23 Vo.  Contact time • bed depth true velocity  -  52 2.2317.82J  • 2.85 seconds,  From eq'n. for Brownian motion (pg. 286, Lapple) 4S  - f URT l ^ t J  3Tf a^NBp  R  - 8.31U ( 1 0 ) ergs/°C (gm. mole)  T  - 293° K  t  " 2.85 seconds  7  - 1.81 ( 1 0 " ) poises 4  N • 6.O64 (lO ) molecules /gm mole 23  Dp - 87 (lO ) cm -6  k  m  - 1.202 AS  > /(U)(8.31U)(10 )(2930(l«2O2)(2.85) 7  J (3)(3.LU) (1.81)(10-4)(6.06U)(10» )(87)(lO"**) a  AS Niow;  3  • 10.7 microns  since the void fraction € • 0.U3 then on the average every void (between  particles is equal to 86$ of the volume of a particle. The volume of a particle  » ^D-, where Dp 3  " 8 9 microns.  Now assuming that as an approximation this void apace be considered similar to a sphere of (0.86)(89) microns diameter then in this volume half the aerosol particles lie further then (0.86)(89)(.793) - 30.4 microns: from 2 the center of void volume and half l i e closer. On the average, then, every particle must travel from this median line to a solid surface, or 89(.86)_ 2 30.4 = 7.9 microns.  The distance a c t u a l l y t r a v e l l e d was 10.7 e f f i c i e n c y should be 10.7  -  135.1$.  microns.  Therefore, c o l l e c t i o n  Data f o r the 3 u l gram f l u i d i z e d bed. Minimum depth Maximum depth  Table H.  Run No.  Through Bed I n l e t pres. P i n Hg. In Hg. —  Ik  r r  23 cms. 28 cms.  Bleed-off Dilution V o l . of K.S. I n l e t pres. flowmeter I n l e t pres. flowmeter Sample Rdg. i n Hg. rdg. i n Hg. i n Hg. ft.3 rdg.in Hg. —  0.500  2k  —  —  0.501  —  3A  —  —  O.U98  lUo  o.5oo  150  UA  —  5A*  —  —  o.5oo  13U  6A*  —  —  0.501  129  8A#  0.30  .35  0.998  65  9A-*  0.80  .35  o.5o  u.95"  1.003  58  10A*  o.Uo  .35  0.30  9.75"  1.000  U9  11A*  o.Uo  .35  0.30  18.75"  1.002  39  12A*  o.Uo  .35  0.40  2.65  mm-*  1.000  U3  13A*  0.90  .35  —  —  2.90  9.95  0.999  69  lUA*  0.90  .35  —  ~  1.50  3.05  1.001  67  l£A*  0.80  .35  —  1.001  71  16A*  —  —  —  0.500  132  17A*  —  —  —  0.U99  138  IB  —  —  o.5oo  lUo  2B*  —  —  —  0  .5oi  126  3B*  —  —  —  o.5oo  136  LB*  0.90  .35  —  1.001  60  $B*  0.75  .35  0.40  2.60  —  1.001  6B*  0.50  .35  O.Uo  3.90"  7B*  o.Uo  .35  O.Uo  8.80"  8B*  o.Uo  .35  O.Uo  17.35"  9B*  0.80  .35  —  —  1.25  10B#  ov?5  .35  ~  —  0.8  LIB*  0.80  .35  12B*  0.75  ,35  13B»  —  —  li|B*  —  —  l5B*  —  -  —  -  —  * indicates second f i l t r a t i o n step was carried out. " indicates inchs of carbon t e t r a c h l o r i d e . ;  0.8  —  U9  0.998  55  —  1.000  U7  —  0.998  U3  11.15  0.991  U.U5  1.000  75 26.0  —  1.000  55  5-.15  1.065  60  —  o.5oo  132  —  O.U98  132  --•  O.U99  129  The method of c a l c u l a t i o n for the A series was similar. - to that of the T and X s e r i e s . runs  The concentration of ester was calculated from the reading f o r  6A, and 16A, 17A. The average of these was taken as the i n l e t mass  loading  and the c o l l e c t i o n e f f i c i e n c y c a l c u l a t i o n as the r a t i o of the e x i t  mass loading over the average i n l e t concentration.  The s u p e r f i c i a l v e l o c i t y  through the bed was calculated by correcting to suitable pressure. Sample c a l c u l a t i o n . Run  No.  mgms. D.O.P. per f t . 3  $k  0.952  6A  0.910  16A  0.93*1  17A  0.983 0.9UU  Avg. f o r run  8A K. So rdg. - 65 mass loading  =  .212 mgm./0.998 f t . 0.213 (11) -  Percent not removed -  3  22.5$  To calculate s u p e r f i c i a l v e l o c i t y . Volume of a i r passing through bed -  16^66 l/m  at 1 atmos. and 70° P. (from c a l i b r a t i o n curves) Avg.  bed press.  Velocity =  =  0.80 .55 = 0.7  29.9 (18.66)  3075  (25.66)  (1000) =  11.82  cm/sec,  J—WJ  (corr. v o l . i n lit./min.) cross ''section  ytec. ) (min.) ( l i t r e ) (sec.)  for Run 9A •  i  •  ble.ed-off reading  k.95 i n CCI4  =  a  5.78 lit./min. at 30.6  r  5.91 lit./min. at latm.  Vol. through bed Velocity  =  18.66 - 5.91  s  29^9 (13.75) )1000) = 3 0 3 " (25.66) (~5o7  in.cC  Hg. ab.  13.75 l i t r e s 8.75 cm/sec.  .181* (100) = 1 9 . 5 $  Percent not removed for Run 13A  Vol. of dilution a i r added - 1*.06 l/m at 1 atmos. Velocity  =  29.9 (22.22) (1000) = I4.35 cm./eec.  3o77  T~5c~)  25.66  Percent not removed  = r :  (0.227) (22.72) = 29.1$  (0.91*1*)  (18.66)  The corrected result was obtained by correcting the over-all collection efficiency for that amount removed by the empty column. Sample calculation Run number 12A Velocity - 3.08 cm./sec. Percent not removed s 13.6 % From figure 8 percent not removed by the empty column • - 70 % 1  Therefore corrected value for percent nob removed by fluidized bed 3  13.6 * 0.70 - j £ 19#  7o  Data for the 651 gram fluidized bed. Minimum depth = kh cms. Maximum depth = 51* cms.  Table I.  Run Through Bed Bleed-off Dilution Vol. of K.S, P Inlet pres. flowmeter inlet pres. flowmeter Sample Rdg, No. Inlet pres. in Hg, i n Hg. in Hg. rdg.in Hg. i n Hg. ft.3 rdg.in Hg. IC  --  2C*  —  3C*  —  Uc*  1.0  5c* 60* 70* 8C*  .95 .70 .65 .65  —»«-  0.500  192  —  —  O.U98  1U0  —  —  —  0.505  132  0.7  —  —  1.000  57  0.70  .80  —  1.001  57  0.70  .65  17.0"  —  .999  Uo  0.70  .65  2.35  i  1.000  38  0.70  .65  2.70  —  1.002  33  —  1.005  55 50  —  —_  —  —  6.U0"  —  90*  1.0  0.70  10C*  1.8  0.70  5.20  2.85  1.000  11C*  2.7  0.70  8.30  U.Uo  .998  12 C*  3.00  0.70  10. UO  5.35  l.ooU  50  13C*  1.0  0.70  —  —  1.000  63  LUC*  —  —  --  —  o„5oo  152  15C*  —  —  —  —  0.501  137  ID  —  —  —  —  0.500  11*1  2D*  —  --  —  —  0.502  121  3D*  —  —  —  —  0.500  1*D  1,0  0.70  —  —  1.000  123 60  5D  2.60  0.70  8.00  1*.00  1.002  U9  2,60  0.70  8.00  U.oo  1.005  58  7D 8D  0.90  0.70  0.80  9D  6D  —  52  ,65  2.U0  —  1.000  0.70  .75  6.20  —  .995  53  —  —  —  —  .5oo  136  IE  —  —  —  —  .5oo  137  2E* UE  —  —  —  —  .502  121  0.9  .65  1.001  62  5E  0.9 0.9 0.9  6E8E 9E 10E 11E*  0.9  .65 .65  .30 .30 .30  2.50" 2.50" 2.50"  .65 .65  .30 .35  2.50? 3.50"  —  . 7.60 5.62u  3  12.65 985  — —  * indicates second f i l t r a t i o n step was carried out. " indicates inches of carbon tetra chloride.  0  —  U3  2*10 U.Uo 3.50  1.000  .998  60 6U  6.00  .998  60  5.oo  1.000  —  0*U99  56 130 128  --  .  O.U99  Table J«  P h y s i c a l data on the Venturis  Venturi  Throat Diameter mm.  Throat Area sq. mm.  Port -^iameter mm.  Port A sq. mm  A  5.69  25.UU  2.87  12.9h  B  3.91  12.01  2.k0  10.92  C  7.00  38.50  2.U0  10.92  D  7.93  U9.32  open  Table K.  ^ata f o r Venturi A _ IQO gms. of gel i n column.  Run No.  Through Bed i n l e t pres. P i n Hg. i n Hg.  Vol.of Samole £t3  K.S.  P-dg.  6F  .15  .10  .502  96  7F  .15  .10  .502  9h  8F  .5oo  139  9F  .SOU  159  r e a  7Z Table L. Run No,  Data f o r Venturi B.  C.  100 gms of s i l i c a g e l i n column.  Bleed--off Through Bed Dilution i n l e t pres. P i n l e t pres. flowmeter i n l e t pres. flowmeter i n Hg rdg.in H . i n Hg. i n Hg. i n Hg. rdg. g  IB  2N 3N  UN  5N 6N 7N 8N 9N  ION  11N 12N 13N IUN  15N 16N 17N 18N 19N 20N 2BI 1M ai-i 3M  mm mm  — — —  — — —  0.25 0.25 0.25 0,60 0,60 0.60 0.60 0.35 0.35 0.35 0.35 .30 .30 .30 .30  lUM  15M 16M 17M 18M 19M 20M  11  neg. it tt " it it ti tt it tt ti — —_  <?«3 0.3 0.3 0.3 0.3 0.3 0.3 0.3  o.U  --  —  0.1 0.1  7.U0" 7.U0"  — —  -— --  9*1 0.1 0.2 0.2 0.2 o.2 ——  —  —  — — — — — —  9,1 0.1 0.1 0.1 0.1 0.1  mm mm  mm mm  — —  — —  >  — —— — —  — —  —  — — — —  — — —  —  — —  ~  1.2 1.2 1.8 1.8  — — —  —  —  — mm  0.5 0.5 0.3 0.3  — — —  Wmmm  — ——  — —  UM  5M 6M 7M 8M 9M 10M II9: 12M 13M  neg. it tt ti  — — —  — — — —  5.U0 5.U0 13.60 13.60 —  — —  15.7'* 2.00 2.00 2.50 2.50  — — — — — ——  — —  — —  — — —  81a 60  ;  --  0.502 0.500 0.502 0.506 .500 .629 ,5U9 .500 .502 .502 .500 .508 .500 .500 .502 .500 .500 .503 .500 .500 .501 .501 .500 .50 2 .500 5oo .501 .500 .502 .500 .500 .500 .502 .500 e  2.60 12.00" 12.005» 5.70" 5.70" — — — --— — — —  Vol.of Sample ft.3  — — — —  —  —  0.9  6.10  18  13.80 13.80  —  B  1.8 -— --  — — — —  K.S rdg  1U9  137 153 1U2 97 106 99 93 87 80  69  70 92  96  100 102 95  99  97 89 156 156 150 139 1U6  97 90 92 93 91 99  98 90 8U  —  .500 .501 .500 .502 .500 .500  69 73 95 100 1U7 1U0  73 D t a f o r Venturi D. 1,59 cm. gap and no cap. 100 gms. of S i l i c a Gel i n column. Through Bed Bleed-off Dilution V o l . of K.S. Inlet pres. P I n l e t pres. flowmeter Inlet pres. flowmeter Sample rdg. i n Hg. i n Hg. i n Hg. Rdg. i n Hg. rdg.in o i l f t . 3  Table M. Run No.  a  f o r runs with 5/8 i n . gap and no cap 1J  0.501  137  2J  0.500 0.502  151 lU9  0.501  IhO  3J —  —  5J*  0.25  neg.  6J*  0.25  7J 8J  UJ  .05  $.60*  0.500  100  .05  5.60  0.502-  109  0.2 0.2  .05 n it  0.503 0.500  98 91  9J 10J  0.2  n  .20  2.U5  .20  2.U5  11J*  0.2  » it  O.U99 0.508  93  0.2  12J*  0.2  tt  13J*  0.2  tt  0.2  1.80  lUJ*  0.2  it  0.2  1.80  15J*  —  16J*  U  12.90« 12.90  1.0 1.0  12J.90 12.90  97 96  0.503 0.500  101  0.5U5 0.500  101  —  0.502  137  —  —  0.500  132  IK  —  —  0.500  131  2K  —  —  0.501  152  3K  —  —  0.507  1U7  ilK  —  —  0.500  I42  5K  0.3 0.3  fie-g. it  ?K  0.3  ti  8K  0.3  tt  9K  0.3  IOK  0.3  6K  0.1  12.it"  0.502  107  0.1  12.ii"  0.500  102  0.500  107  0.508  100  II  0.05  6.00"  0.500  110  it  0.05  6.00?  0.500  103  0.500  LUO  11K * indicates second f i l t r a t i o n step was carried out. "indicates  111  inches of carbon t e t r a  chloride.  Data f o r l e n t u r i D 1.59  Table N.  cm. gap with plexiglass cap  100 gms of s i l i c a gel i n column.  it  un No.  Through bed Inlet pres. P i n Hg. i n Hg.  Bleed-off I n l e t pres, flowmeter i n Hg. rdg.  Dilution Vol.of I n l e t pres. flowmeter Sample i n Hg. rd. i n o i l ft3  K.S, rdg,  1L*  —  —  —  —  .501  129  2L#  —  —  —  —  .5oo  lUo  3L*  —  —  —  —  .5oo  142  liL*  0.2  neg.  —  —  .500  100  5L*  0.2  tt  —  —  .503  100  6L*  0.25  re  7L*  0.25  it  —  8L*  0.25  it  o.5o  5.70"  .5011  111  9L*  0.25  n  o.5o  5.70"  .503  liU  10L*  0.25  it  1.25  2.00  .503  107  ILL*  0.25  tt  1.25  2.00  ,5oo  . 113  —  .5oo  129  IP*  1.10  10.2  .502  110  1.10  10.2  .5oo  90  2P*  —  —  .5oo  139  3P*  —  —  ,5oo  130  UP*  0.25  neg.  1.2  12.h  .501  85  5P*  0.25  n  1.2  12.U  .U99  78  6P*  0.25  tt  1.2  12.U  .509  90  7P*  0.20  it  —  —  .500  109  •;8P*  0.20  n  —  —  .500  101  9P*  —  —  mm *-  —  .500  133  10P*  0.2  Neg.  o.o5  6.10"  .5oi  116  IIP*  0.20  1  0.05  6.10J?  «502  120  12P*  0.20  f  0.05  6.10"  .500  112  13P*  0,20  0.05  6.10"  .5oo  119  * indicates second  f i l t r a t i o n step was carried out-  it indicates inches of carbon t e t r a chloride.  7J~  Table 0.  s  o l i d s flow data f o r venturi B. 100 gms. of s i l i c a g e l i n column.  Run No.  i n Hg.  Wt. ,of gelgms.  Time seconds  Manometer 1A  2  2A  16.2  16.0  12.9  9.5  30  1  1 16.0  2  16.0 1 ; . ^  16.2  16.0  12.9  8.3  30  3  16.0  16.2  16.0  12.9  8.9  30  u  11.0  10.2  11.5  10.0  5.6  30  5.  11.0  10.2  11.5  10.0  6.3  30  6  11.0  10.2  11.5  10.0  6.3  30  7  10.0  8.3  9*5  8.0  2.5  30  8  10.0  8.3  9.5  8.0  1.9'  30  9  10.0  8.3  9.5  0.0  1*1  60  10  7.5  6.0  7.5  5.7  3.0  60  11  7.5  6.0  7.5  5.7  3's.O  60  12  7.5  6.0  7.5  5.7  2.8  13;  3.5  2.9  3.5  2.7  2.0  li;  3.5  2.9  3.5  2.7  1.7  60  15  3.5  2.9  3.5  2.7  2.U  60  16  17.0  17.8  16.5  17.0  7.1  60  60 60  17  17.0  17.8  16.5  • 17.0  8.0  60  18  17.0  17.8  16.5  17.0  7.2  60  19  same ias 18 plus  15.1  60  20  d i l ' n flow = 12.2 divisions  15.U  60  21  at 1.2 i n Hg.  15.3  60  Table P. SolxdSj flow data f o r venturi C.  No.  100 gms of s i l i c a gel i n column. Manometer i n Hg. Wt. of 2 gel gms. 1 1A 2A  1  5.5  il.l  5.0  3.9  3.2  60  2  5.5  il.l  5.0  3.9  2.8  60  3  5.5  4.1  5.o  3.9  3.0  60  U  11.0  8.9  10.0  8.6  ii.2  60  5  11.0  8.9  10.0  8.6  3.7  60  8.9  10.0  8.6  3.6  60  12.2  5.1  60  ii.6  60  ii.il  60  5.8  60  6  •  11.0  lii.O  7  lii.O  13.ii  8  lii.O  13.ii  lii.O  9  lii.O  13.U  lii.O  10  17.5  11  17.5  12  17.5  13  17.2 17.2 17.2  at  =  12.2 16.6 16.6  6.2  60  17.0  16.6  5.5  60  10.8  60  11.2  60  10.9  60  12,0 d i v .  1. 1 i n . Hg  12.2  17.0  same as 12 plus d i l ' n flow  15.  17.0  .  time seconds  77 Table Q.  Solids flow data f o r venturi D. 100 gms. of s i l i c a g e l i n column.  Run No.  1  1  2.5  2  2.5  3  2.5  U  8.5  5  8.5  6  8.5  7  Manometers 14 2  2A  Wt. of gel gms. '  Time seconds  2.5  1.7  U.o  15  2.5  1.7  U.8  15  1.9  2.S  1.7  U.2  15  5.7  8.0  5.2  19.5  15  8.0  5.2  19i7  15  5.7  8.0  5.2  19.0  15  11.0  7.3  io.5  7.0  22.3  15  8  15.5  13.7  15.5  n.5  22.U  15  9  15.5  13.7  i5.o  11.5  23.2  15  10  15.5  13.7  i5.o  n.5  23.2  15  11  20.0  17.lt  20.0  15.8  25.2  15  12  20.0  17.4  20.0  15.8  25.5  15  13  20.0  17.4  20.0  15.8  2U.9  1.9  22.0  lU  21.8  15  same as 13  16  plus d i l ' n flow of 13.7 i n o i l  17  at 1.1 i n Hg.  18  4.0  3.1  4.0  19  4.0  3.1  20  4.0  3.1  23.8  15  IS 15 15  21.5  15  2.9  12.9  15  4.0  2.9  12.2  . 15  U.o  2.9  13.0  15  Table R.  20 Drum Divisions  Aerosol Measurement data.  =  1 micron.  1  16  17  18  16  19  19  Iii  17  16  15  10  2  18  19  18  14  17  20  20  17  21  15  17  3  18  19  17  19  17  17  25  19  19  21  16  k  , 17  111  13  Iii  16  17  16  15  19  17  20  5  16  23  19  15  11  16  19  16  111  11  20  6  17  16  17  17  21  19  lli  22  16  19  15  7  19  16  17  15  18  10  Iii  12  12  27  17  8  20  17  15  19  15  19  17  19  17  12  22  9  19  19  20  16  18  16  18  19  16  16  22  10  2h  20  16  16  19  16  16  16  19  17  14  11  Ik  12  21  18  17  15  19  21  15  19  16  12  17  20  14  18  16  17  17  19  17  19  17  12  18  18  18  15  19  12  10  19  26  16  19  111  19  19  19  19  15  19  18  17  16  17  15  15  16  17  15"  26  15  15  16  13  19  18  18  16  16  15  17  17  18  16  15  16  20  16  16  17  17  19  15  18  1$  17  17  17  21  17  20  18  19  13  19  17  19  Iii  17  18  15  19  18  19  13  20  20  17  17  16  15  20  Iii  15  17  20  17  16  16  18  19  16  19  17  18  15  16  378  360  3U1  326  336  359  350  336  3hi  over a l l t o t a l -  38/4O  21  20  total3$8  3u9  average p a r t i c l e s i z e -  38ii0 20(221)  -  0.869 microns  APPENDIX A. Solutions required for a n a l y s i s : A.  2.5$ sodium hydroxide ( 4 ) . Dissolve 2.5$ by weight o f pure sodium hydroxide i n 95$ ethanol. Add  approximately 1 milligram o f sodium carbonate. B«  Make s o l u t i o n fresh d a i l y .  2.5$ hydroxylamine hydrochloride(4) Dissolve 2.5$ weight of pure hydroxylamine hydrochloride i n 95$  ethanol. C. c  Make fresh d a i l y .  Modified s o l u t i o n A. (5) . Dissolve O.U gms o f i r o n i n 20 ml o f 1 to 3 n i t r i c acid (1 a c i d to 3  water), add 15 ml o f 70$ perchloric acid and heat to copious fumes o f perchloric acid.  Cool and transfer to a 100 ml volumetric f l a s k with the a i d o f  4O ml 5/water added from a pipette. -Add 10 ml o f cone. n i t r i c acid and d i l u t e to the mark with 70$ perchloric a c i d . Make a 1$ solution o f t h i s i n 95$ ethanol. The concentrated solution i s good i n d e f i n i t e l y . The d i l u t e solution i s good f o r a week.  APPENDIX B: Formula f o r  di-n-octylphthalates  0  CEj - CH t -C - 0 - CH - CH - CHj - CH - CH 3  2  a  3  -C - 0 - CEj - CH - CHjj - CH - CH a  0  CHj - CH  3  3  APPENDIX C. Flow Meter Calibration Data: Manometer 1  -  meters flow to preheater  Time minutes  ft3  Scale Rdg, 1 d i v . = 1/L0 W  cfm  Liters " minute  3  0.312  5.5  0.101+  2.95  U  0.k2h  io.5  O.lkl  fc.Ol  3  0.773  17.5  0.191+  5.50  3  0.765  2U.5  0.255  7.23  3  0.861  33.5  0.287  8.13  3  0.996  U3.5  0.332  9.1+1  3  1.107  53.5  0.369  10.U5  3  1.180  61.5  0.393  11.15  3  1.252  68.5  0.1+17  11.80  Temperature  70° F.  -  /  Pressure ~ 1 atmosphere  Metering fluid - carbontetrachloride  Manometer 2 -  Metered fluid - a i r  meters flow to m^ucleation chamber  Time minutes  fta  3  0.262  3  cfm  Liters minute.  1+.5  0.087  2.1+7  0.1+20  10.5  0.11+8  3.86  3  0.1+79  13.5  0.1597  U.53  3  0.600  20.5  0.200  5.67  3  0.700  27.5  0.233  6.60  Temperature  -  Scale Rdg. 1 d i v . " 1/1°"  70° F .  Pressure - 1 atmosphere  Metering fluid - carbontetrachloride  Metered fluid - air  FIGURE  23  CALIBRATION  CURVE  FOR  MANOMETER I : TO  PREHEATER  2-5  0  '  2  2,5  FIGURE 2 4  !  I  3  3.5 LITERS  CALIBRATION  1  I  4 4.5 PER MINUTE OF  CURVE  FOR  L  3  1  5.5  L  1  6.  AIR  MANOMETER  2 '. TO  NUCLEATION  Manometer 3  -  Time minutes  ft  bleed o f f - manometer Scale Rdg. 1 div.» l / 1 0  3  rt  cfm  Liters minute  Inlet press i n . Hg.  3'  .188  0.6 +  .063  1.78  0.10  3  .319  1.4  +  .106  2.9U  0.20  3  .31+5  1.7  +  .115  3.25  0.25  3  .U23  2.3 +  .ll+l  3.99  0.1+0  3  .530  4.0  +  .177  5.01  0.60  2  .U32  5.8 +  .216  6.12  0.80  2  .572  10.2  +  .286  8.09  1.1+0  2  .672  11+.1 +  .336  9.50  1.90  2  .422  • 0.65 t  .211  5.97  .80  2  .668  1.65 A  .331+  9.1+5  1.95  2  .811  2.25 A  .406  11.1*5  2.60  2:  .918  2.85 A  1-459  13.1  3.20  Temperature  -  70° F.  Metering f l u i d  + carbontetrachloride A mercury  Manometer 1+ •  d i l u t i o n manometer  Time minutes  f t  3  Scale Rdg. in.Oil  Metered f l u i d  cfm  Liters minute  3  0.106  1.10  0.0353:  1.00  3  .199  2.80  0.0662  1.88  3  .259  1+.55  0.0865  2.1+5  3  .311+  6.55  0.101+8  2.97  3  .361  8.35  0.1202  3.1+1  3  .1+11  11.90  0.1369  3.88  3"  .1+50  13.1+0  0.150  1+.25  Temperature  «  70° F .  Pressure  Metering f l u i d - draft gage o i l  S.G- - .826  -  1 atmosphere  Metered f l u i d  - air  - air  LITERS  PER  MINUTE  OF  AIR  I  FIGURE 2 6  CALIBRATION  CURVE  DILUTION  FOR FLOW  MANOMETER  4  

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