'thossible use in the removal of oil mists and hydrocarbon vapors. '5* A controlled flow of oil was injected into a heated n1cke1 reaction '¥radsorption 1sotherms for this material ;m_ . L .‘f"flé‘fi. N . e Lo e e OAK RIDGE NATIONAL LABORATORY ' operated by umou CARBIDE conponAnon - u s ATOM!C ENERGY commssuon ', c:::s::z PRITIS ORNI. TM- 1623 'copvno,i Jffiflf: | ; RG S 5’ O DATE - Sept 7, 1966 TESTS OF VARIOUS PARTICLE FILTERS FOR REMOVAL OF | OIL MISTS AND HYDROCARBON VAPOR R "B, F. Hltch R.;G Ross, H. F. McDuffie ABSTRACT Various filter and adsorbent materials were examined for = é—'-— ivessel to cause vaporization and some cracking of the 011 Helium ,flowing through the reaction vessel carried the 011 mist and hydro— : Ocarbon vapor through a filter system. Filter effectiveness ‘was .;Irdetermined by the use of a Perkin-Elmer Hydrocarbon Detector,_ o grav1metric analysis, and ‘gas chromatographic analysis., Good removal of mists was achieved by the use of a. combination of _ | ;'felted metal fibers and ceramic fibers in a configuration proposed I;:afor use in the MSRE._ Granulated charcoal removed hydrocarbon _'7{fvapors (Cs ‘and above) 1n a manner consistent with the established LEGAL NOTICE | This report was prepared as an account of Government sponsored work. Neither the United . - | Btates, nor the Commiasion, nor any person acting on behalf of the Commiasion: : A. Makes any warranty or representation, expressed or implied, with respect to the accu- racy, completeness, or usefulness of the information contained in this report, or that the use’ of any information, appantus met.hod, or proceas disclosed In this report may not infringe R privately owned rights; or . B T ’ B. Assumes any liabilities wlth respoct to the use of, or tor damages resulting [rom the o use of any information, apparatus method, or process disclosed in this report. : AS used in the above, *‘person acting on behalf of the Commisajon® includes amy em-- ployee or contractor of the Commission, or employee of such contractor, to the extent that - such employee or contractor of the Commisajon, of employee of such contractor prepares, disseminates, or provides sccess to, any information pursuant o hia employment or eontnct . with the Commission, or his employment with such dontractor. : ' RELEASED FOR ANNOUNCENERT | _ This document contoms mformahcn of a prellmmcry nature and was prepored ' pnmanly for internal use ‘ot the Oak Ridge National Laboratory. It is subject rto revision or correction cnd therefore does not represent a final report.:_ S - fihadmvsrr‘Dc_&awuwn}, TIGNS GF PRZENT mmm Lotuve& G A T THEARC. M2 RS - /ck4 b i o i i ¥ i i ‘ i i@ i i { f z LEGAL NOTICE This report was prepared as an account of Government sponsored work. Neither the United Stat-as, nor the Commission, nor any person acting on behalf of the Commission: A. Makes any warranty or ' representation, expressed or ‘implied, with respect to the accuracy, completeness, or usefulness of the information contained in this report, or that the use of ony information, apparotus, method, or process disclosed in ihls report mdy not infringe privately owned rights; or : B. Assumes any liebilities with respect to the use of, or for damages resvlting from tho use of . any informaticn, apparatus, method, or process disclosed in this report, As used in the above, “’person acting on behalf of the Commission®” includes any .mployea or contractor of the Commission, or employee of such contractor, to the extent that such employse - or contractor of the Commission, er smployse of such contractor prepares, disseminates, or provides access to, any information pursuant to his employment or contract with the Commission, or his smployment with such contractor, ? Y + CONTENTS P Page _ ABSTRACT. . + &« v v o v v v e o v v v o 1 INTRODUCTION. . « « o o o v e e e e u . 4 PROCEDURE © + + ¢ ¢ ¢ o o o o o v o o « . 4 OIL MIST FILTERS. . . . . . . e e e T 3.1. General DeseriptiOn R 7 - 3.2, ExperimentallData ¢« o o w » ; . o » 7 - 3.3. Experlmental Data After Alterifig 0il InJectlon ¢ o e s 8 a8 e o o o 9 CHARCOAL TRAP EFFICIENCY. . . . . . . . . 12 4.1. Charcoal Saturation with Hydrocarbons 13 4.2. Temperature Dependence of Hydro- ‘carbon Adsorption on Charcoal . . . 13 TESTING OF MSRE PARTICLE FILTER . . . . . 19 5.1. Pressure Drop Data. . c e e e .. 19 5.2, Pressure Dr0p Data of Felt Metal | at Elevated‘Temperatures. c s+ e« . 23 ACKNOWLEDGEMENTS. . . . . . . . e e . 25 1. INTRODUCTION c ) u L. ‘ One of the problems encountered during the early stages of power Operation of the Molten Salt-Reactof»EXperiment wéé that éome valves and filters in_tfie‘offfgas-syStem becéme‘ plugged. The plugs were analyzed and found to be of organic COmposition. | - | One possible éource of-organic material was the oil used to lqbricate the salt circulating pfimp; If'indeedjthe pump were leaking oil inté the pump bowl, the maximum!credible" Ieakage fiould be in the range of ls‘to 20 cc pérday;' This experiment was designed to‘simuiate:the consequences ofjthis maximum expected oil leakage and to test various filter and adsorbent materials for removal of oil mist and hydrocarbon vapors under these conditions. o & 2. PROCEDURE A complete flow diagram of the-appgratus is Shown in’." | - Fig. 1 and a pictfireas Fig. la. - | . L Gulfspin-35 oil is used to lubricate thelMoltén Salt | Reactor pump; this same o0il was used in our expériments. The ' oil was injected by a motor driven sjringe connected byfa capillary tube to a heated.reaction vessel; .The injection 'rate was 0.67 cc,pef hour. | | | Simulating MSRE off-gés flow condifions, helium was passed through the system at 4 liters per minute. The nickel reaction vessel temperature was about 600°C, The gas effluent from the filters A, B, C, D, and E ORNL DWg. 66-9447 Motor Drwven SyR\NGE | #t] CHARCOAL l $#2 CORRCOAL VENT F S-3 Fig. 1. O0Oil Injection and Filtering Apparatus a¥® o | ‘ | o of » - . o) &i W+ w - i Fig. 1a, 'Picture ~N PHOTO 83330 of 0il Injection and Filtering Apparatus URY B -l » | passed through two, charcoal traps f111ed with PCB 6X16 ’ . charcoal A Perkln-Elmer 213 Hydrocarbon Detector, prov1ded by the Analyt1ca1 Chemistry D1v1s1on, was used to measure the ~hydrocarbon levels at_three.p051t10ns (S-l, S—Z, S-3) shown on the flow diagram. GaS‘samples,were taken periodically at these same three p051t10ns for subsequent chromatographlc analysis, Pressure drop measurements were made us1ng Hg and H,O manometers. Readlngs were taken each half hour. 3. oIL MIST FILTERS 3.1. General Description lelted t1me necessitated that the 1nvest1gat10n of filter materlals be conflned to those ea511y obtainable. Materials tested were coarse nickel wool, Supreme #1 steel “wool, Supreme #00 steel wool Pyrex glass wool, Fiberfrax and a M-S—A a1r.11ne Ultra Filter. | Flberfrax showed an appreclable pressure drop when packed 1nto the glass U- tube traps. This was tfie short fiber varlety whlch packed very tlghtly when loading the traps._ Because the pressure drop was in excess of 8 psig, thlS material was not “ :tested However long f1ber Flberfrax proved to be satlsfactory;t IB,ZgK_Experimental Data,_ '3.2.1. The first. two experlments were performed us1ng | coarse nickel wool 1n trap A and Supremet#l steel wool in traps B and C. The-data summarized iinable 1 show thiS'trap assembly removedeS%;of the total oil injected into the Tabhle 1, Efficiency of Filter Materials Tested . Trap A Trap B Trap C Total 0i1 Total Oil Run Length of Filter Wt. of 011 TFilter Wt. of 011 Filter Wt. of 0i1 Removed Injected por cent of # Run (hrs) Material Removed Material Removed Material Removed () (g) 0il Trapped 1,2 6 Coarse N1 ' 0.690 #1 Supreme (0,878 #1 Supreme 0.501 2,069 3.740 55 wool (1) ste?l)wool steel wool z » 3 13 Coarse ¥i 1.735 #00 Supreme 3.428 #00 Supreme 0.749 5.912 7.410 80 wool ste?I)wool steel wool - ' 3 4 18 Coarse N1 3,749 Pyrex glass 5,440 Pyrex glass 0.000 9,189 10.090 91 ' ‘ wool wool wool S ‘ 5% 23.5 #00 Supreme 5.341 Pyrex glass 3.792 Pyrex glass 0.278 9.411 13.400 70 ‘ steel wool , wool wool ' ~ : bA* 22.6 #00 Supreme 4.929 Pyrex glass 4.188 Pyrex glass 0.123 9.240 12.882 72 : _ . steel wool wool wool ' 6B* 31.6 #00 Supreme 6.892 Pyrex glass 5.374 Pyrex glass 0.001 12.267 18.012 68 i sthel wool wool wool o T* 88 Trap A, B, and C replaced by MSA Ultra Filter using 47,486 47.486 50,160 95 7930 cartridge ¢ *Thase runé were made with oil béing injected into dip-leg. (1) Surface area of 0.016 square meters per gram, (2) Surface area of 0.032 square meters per gram. {(3) Surface area of 0.047 square meters per gram. ~ at . - at point P as shown on the flow d1agram in Flg.rl.. This entry lp01nt was changed to p01nt P so that the oil entered dlrectly 5_t1nto the;stream\of,flowlng helium and downgthe_dlpeleg of the reactlon vessel However, in the first few runs a portion of the oil was probably held up on the walls of ex1t lines. - '3.2.2( .Experiment #S-utilized the same-Coarse nickel wool in trap A. Trapsz.and_C"were filled with Supreme #00 steel wool. Eighty percent of the total oil injected was ‘removed with these traps- 3.2.3. Experiment #4 used coarse nickel wool in trap A and Pyrex glass wool 1n traps B and C.' Although this run was of_greater duratlon_than prev1ous ones,.no_increase'in weight Wasrfound‘in trap C. Ninety;one per cent of-the oil injected was removed by thlS trap assembly. 3.2.4. The follow1ng summary indicates the amount of oil retained per gram_of_fllter material used in experiments 1 through 4. Expt. # Trap A ‘Trap B Trap C 1and 2 .020 .066 . 048 3 049 .244 .078 4 r'.106r*;—;[;;754 -0 '77”3.3.; Experimental Data After Alterlng 011 Ingect1on To obtain better cracklng, the oil entry to the react1on ',stessel was altered. In experiments 1 through 4 the 011 entered reactlon vessel. U51ng this method of 1nJect10n, the hydrocarbon level at 10 the three analysis points S-1, S-2, and S-3 rose to about ten times previous levels. Obviously, much less cracking had occurred in experiments 1 through 4. 'The average hydro- carbon levels are summarized below: . - \._ Expt. # Analysis Analysis - Analysis Point S-1 Point S-2 Point S-3 l - 4 75 ppm ‘ 35 ppm : 22 ppm 5 -7 715 ppm , 360 ppm 285 ppm ; 3.3.1. Traps for experiments 5, 6A, and 6B contained Supreme #OO steel wool in trap A, and Pyrex glass wool .~in traps B and C. 0il recovery ranged from 68% to 72%:for.this trap assembly. More efficient cracking of the oil resulted in a decreased oil recovery. It should be noted that in each of these runs only a small portion of the adsorbéble oil migt reached trap C as shown in Table 1. f 3.3.2. Experiment 7 investigated the efficiency of a commercial filter assembly. A M-S-A air line Ultra Filter as shown in Fig. éfwas used. The particulate filter_element is molded of a cellulose matrix with glass microfibers added rto present a large capturing surface. The caftfidge holder.. is equipped with é drain plug through which 1iquids can be - removed periodically. - The M-S-A filter assembly was‘instélled in our apparatus, replacing traps A, B, and C. | This filter assembly was the mbst efficient fiiter material tested, retaining 95% of the oil injected into the s . N . |- - 5 . \ ! . - - <~ - ’ - 3 4 " 7 = 3 ~ . 12 reaction vessel. All of the trapped oil mist was retained in the filter element, no liquid was present in the cartridge holder. 3.3.3. The foilowing'summary indicates the grams of oil mist retained per gram of filter material tested. ‘Expt} # - Trap A Trap B'_ Trap C 5 0.319 gnm 1.365 gm 0.049 gm 64 0.295 1.243 0.023 65 0.412 0.925 no wt. gain 7 1;700 e | - - 4. CHARCOAL TRAP EFFICIENCY The charcbal traps used‘in'ogr experiments were 1l-in. I.D. glass Pyrex pipe packed with about 12 inchés of PCB 6X16 charcoal. | Under reactor conditions, the decay of fission products is expected to raise the temperature of a charcoal trap’of the above dimensions to abofit 100°c. Consequently, charcoal traps were kepf at a\temperature of 100°C during our eiperi- ments. | A point of interest was the amount of hydrocarbons necessary to saturate a known amount of charcbal at 100°cC. Data for this investigatioh were obtainéd'simultanéously with the filter material tests previously described. | Charcoal trap #1 shown in Fig.-l was filled with a known amount of charcoal. Sample'points S-1, S-2, and S-3 were wi -~ monitored with the hydrocarbon detector. .Saturation was 13 assuned when the hydrocarbon-level‘at S-2 started approaching _.the level of S 1. 4.1. Charcoal Saturatlon w1th Hydrocarbons Figure 3 summarlzesrthe tworexperlments carried out. . The first experiment madeuse of a packed_bed‘of'about 3 inches of charcoal in a glass trap;,“The'weight of charcoal was 'approx1mate1y 6.0 grams per inch. The first evidence of satura- - tion occurred at a total t1me of 30 hours. A second ‘test with ( about 6 1nches of charcoal reached saturat1on in about 60 hours. The hydrocarbon_levelratgs-l and S~2 averaged_700 ppm and 425 *ppmi(CH4 eq.) respectiveiy prior'to trap saturatiOn. The 3-1n. trap was analyzed after it became saturated . R "and the results are shown 1n"Tab1e 2. Thls data 1nd1cates that as the heaVier-hydrocarbons were more strongly adsorbed in the top of the trap, the 11ghter hydrocarbons were forced i;t0'the bottom. "Breakthrough" occurred when the C; hydro- carbons were forced out., Table 3,contains gas samples taken. | before and after hydrocarbon saturatlon. /4;2. Temperature Dependence of Hydrocarbon Adsorptlon o L fm" ‘on Charcoal ) Adsorptlon of hydrocarbons on. the charcoal 1s a functlon -fof charcoal temperature as shown in Flgs. 4 and 5. Upon :“?coollng charcoal trap #2 from 100°C to 25°C the he11um efflu- '.“ent to the trap was lowered to approx1mately 40 per cent of ) the or1g1na1-hydrocarbon.concentratlon. Coollng from 100°C ORNL IWG. 66-9448 ) “~ O o Y Hydvecarboms wmeT: Re Anoued by Chavecoar Zree £, %, 3 _O o o o o S o ‘ o & o -rl'Ne- ( Rowrs) Fig. 3. Hydrocarbon Saturation of Charcoal Trap #1l ro Y1 *h C ( 15 ~ Table 2. Hydrocarbons Adsorbed in 3-in, Charcoal Trap Concentration, Wt. % In Taches <% G G G Cuao >C, Total 0.0 - 0.5 0.5 0.3 0.3 0.3 2.1 14.3 17.8 0.5 - 1.0 0.3 0.2 0;4 1.6 5.6 9.4 17.5 1.0 - 1.5 0.3 0.3 1.4 4.0 4.5 3.1 13.6 1.5 - 2.0 0.2 0.8 4.2 3.3 0.6 0.3 9.4 2.0 - 2.5 0.3 1.9 2.6 1.0 0.1 0.1 6.0 2.5 - 3.0 0.2 2.3 1.1 0.3 0.0 0.0 3.9 0.4 2.7. 0.3 0.1 0.0 0.0 3.5 16 Table 3. Analysis of Gas Samples Taken Before and After Hydrocarbon Saturation of Charcoal Trap (ppm by Volume) - Isomeric Hexenes Before: | After Components Sample Sample Sample Sample Pt. S-1 Ptf S-2 Pt. S-1 Pt. S-2 Methane 25 30 16 28 Ethane 4 6 3 7 'Ethylene 70 95 41 80 Propylene 33 40 20 41 Butene-1 7 12 7 12 Isobutylene 3 3 4 4 - Cis-Butene-2 4 8 5 8 2-Me Butene-1 4 - 8 10 Pentene-2 1 - 2 2 rBranched Hexenes 5 - 1 3 Hexene-i 3 - 4 37 1 - 1 6 " 5% PPM . {"Y?’*#Cfl'-'*ffi'('é Hy 2g-) I -‘—""?"r“i T#24p, “ S . - ' ORNL ING. 66-9449 {0 "'\';.:uu, L Hvo) '“ Fig. 4. Hydrocarbon Adsorption on Charcoal at 25°C and 160°C | LT P/Q/L/’ /lyJVOD"FAW (;F’q ‘1') W ENT ’TJ’ffiM AN &oo ~3 9 . o, o0 At @ Time CHvs) Fig. 5. Hydrocarbon Adsorption on Charcoal at 25°c, 75°C, and 100°C. . 66-94 ST (7. ] 2 ne _19 to 75°C lowered the concentration to 70%. When the trap was returned to 100°C :after each cooling dycle the hydrocarbon content rose sharply thenreturned to its original.level. 5. TESTING or MSRE PARTICLE FILTER -Traps-A,-B,.and C mere“repiaced with a prototype of the MSRE particle filter shown in Fig. 6. This filter was prepared by personnel of the Reactor'Division. The filter consisted of two‘Huyck_stainless'steel felt metal filters and a chamber filled with long fiber:Fiberfrax. Pressure drop measurements were made to determlne the maxXimum AP after the felt metal filters were saturated w1th 0il mist. Measurements were made using Hzo-and Hg manometers, A further test was performed in which the felt metal filters_were welded inside,a stainless steel pipe as shown in Fig. 7. This assembly was placed inside a tube furnace and tests were conducted at various temperatures. L ,5.1.77Pressure Drop Data Flgure 8 shows the pressure drop data obtalned from the - MSRE partlcle f11ter test., After ‘24 hours the pressure 'g»remalned constant at 2 7 psig.' Attempts to blow the oil off the felt metal fllters, by suddenly 1ncreas1ng the flow rate .'of he11um to 8 liters/mln, were not successful The AP ‘would -drop sl1ght1y, ‘when the flow rate was returned to 4 11ters/m1n, but returned to its former level in less than 5 m1nutes. The felt metal fllters were removed from the system and a pressure drop across the Fiberfrax alone was determined. The 20 ORNL IMG. 66-9451 - ‘ — ! quax Girss -7 4 - To. . K / ~ Pire to N\fiNOMfl.‘\ev n ‘; L s b Anvene e . . l - e o — “e\'\“"« i "’g e . .;._ v_— w..;.mz-__ ———— Eaotrane b s 2 o e “;A..\-p_!( . “v..,c( . -T‘\p'— 215 (Convie) ] TyPe 0¥ (,FUJ&)‘ Fer\ v Mervol Filldes Cer= Metal Filtev FJ.g 6. Sketch of MSRE Particle Filter Prototype w1y ol o 9 - | ' | ORNL DWG. 66-9452 ‘ S : ' i'L@flG ' 1 : o o b . . ‘ .7 y oo e Eno fFares [§ Tik, » : ‘!' | _,/ - - ! | | 4 A . ,‘e / 2% _4aE"ID - ;;\\ s 5 . 9 4" seh 40 - Felt Memar Dises I,—, r/ Fire 1y ' ' 4- A 7 1 / 7 ?~N~\/MDD xm:f”vme l e wELL | Fig. 7. Felt Metal Fllter Assembly Used At | Elevated Temperatures ORNL, DWG. 66-9453 3 . 24 22 FPessare Prop (P’I) : * Lo 1o ] | e (Hv) Fig. 8. AP Across Prototype at MSRE Particle Filter 23 pressure dropiwas'0.0IZ psig'and»remained constant over a 20-hr period. . 5.2, Pressure Drop Data of Felt Metal at o ' - Elevated Temperatures ‘A filter assembly with the coarse and fine felt metal filters welded in a stalnless steel pipe was fabricated as shown in Fig._9. -The assembly was placed in a 5-in. tube furnace. It was desirable to measure the AP of the felt metal filters atfelevated temperatures, since during reactor operations, the decay of fission products would possibly raise the temperature of the fllter assembly. | | Measurements at various temperatures were reproducible as shown in Fig.p9, However, the maximum AP at 25 ¢ was 0.45 p51g compared w1th 2.7 ps1g measured in the previous experiment. | DOP measurements conducted by the Reactor Division on the prototype-of'the MSRE particle filter showed'it‘to be 99. 98%:efficient. The welded filter assembly, when tested, was only about 95%>efficient. Although there was no visible ev1dence, cracks may,have been present in the welds of the Welded.filterdassembly./ _ Thirty hours at 25°C were required before the felt metal filters became saturated with oil mist. The transition'to the maximum AP required oniy about one or two minutes. Upon reaching maximum AP at room temperature, heat was applied to the filter assembly. At a temperature of 150°C the AP 2:35«.@ bVOF (p‘s--zj Las - - 1o o T ime ( Houre) 24 ORNIL, DWG. 66-9454 Fig. 9. AP of Felt Metal Filter 25 decreased sharply, returningaalmost to the minimum. When the temperature was raised to 400°C and 600°C the AP rose slightly in each Case but gave no indication of plugging. The rise in AP associated with a rise in temperature can probably be attrib- uted to an increase in the viscosity of helium. The viscosity of helium at 25°C 1s_180 micropoises,’and at 600 C is 405 'micropoises. < A total of 230 grams of Gulfspin-35 oil was inJected into the heated reaction vessel during the prev1ous1y described experiments. Upon termination of the experlments the reaction vessel was cut apartforyvisual inSpection. The vessel con- tained 0.5 grams of dry Carbon; no evidence of any liquid hydrocarbons Was found., | | The welded felt metal filter assembly was also cut apart; again no liquid hydrocarbons were found 6. ACKNOWLEDGEMENTS 6.1. Excellent coOperation and much assistance ‘was received from Messrs.-A S Meyer, C. M. Boyd and A. 'eHorton, of the Analytlcal Chemistry Division ‘who supplied .and installed the hydrocarbon gas analyzer, assisted us with cflthe 1nterpretation of the results, and analyzed many samples _of gas and charcoal by the gas chromatographic procedure. 6 2. Continuous operation of the apparatus over the .period of many days was made possible by the MSRE Operations section through their assignment of personnel for-taklng data during the:evening'and night shifts. 26 | 6.3. The close cooperation and frequent discussions with D. Scott,'Jr;, were ihvaluable in guiding the investi- gation in directions which were useful for the application ‘of filters to the MSRE off-gas system. g 4 > / 1. 3. 4. 5. 6. 7. 9. 10. 11. 12. - 19. 205 - 21. - 22. 23, 24. 25. 27. 28. 29, 30, - 31. s 33, 34-35. - 36. "37;39{ 40, 41, 27 DISTRIBUTION G. M. Adamson C. F. Baes, Jr. 'S. E. Beall E. S. Bettis F. F. Blankenship E. G. Bohlmann R. B.‘Briggs- W. H. Cook W. R. Grimes A. G. Grindell P. N. Haubenreich' B. F. Hitch ‘A. D. Horton P. R. Kasten S. S. Kirslis 'R;;B.'Lindauer H. G. MacPherson H. F. McDuffie ‘A. S. Meyer, Jr. 'R;,L.»Moore .R;~J,*Ross D. Scott, Jr. ~A. N, Smith P. G. Smith uflf_R;eTallackson RAIE;Thoma M. E. Whatley | fCentral Research L1brary ‘Document Reference Sectlon,‘ 'Laboratory Records | Laboratory Records, ORNL R. C. ORNL Patent Office 28 EXTERNAL DISTRIBUTION 42. Research and Development Div., OR - k3-57. DTIE, OR c\h . e ’[: )4‘ | ’ For