f: 3 ; 1'. '1 J " 4’— L.‘ 7 J'— |——— a ”i 114 "THS 43.. . r7 AN EXPERIMENTAL STUDY OF ACTIVATED CARBON IN INDUSTRIAL ~ WASTE TREATMENT Thesis for the Degree of B. 5. Allan J Kronbach 1935 $2,353,: _ cckv'v'g'; ”35.5.: r A .a V :- ~ A 12:; ~fw’” ‘1 - .:..~'.‘ Jr " :r‘iJVz‘".t NI; ~ 4'3"“ ‘ . 33,1 .23%,«>£1¢=.-.y ’*~'t?~.->rr—:vic art. 1 5 ', «$3M; figswujs‘: ‘ . .14. y? a! ‘, ‘4: gnu-fl 1‘ I... , ‘2 4 ‘6“? "V*V*.‘1"—'§-$§;P 3:31”? m. .'.+:‘ '- ~c * '- n, ' , I 'I -. l’lgjlb‘c (:‘T‘a'y gd‘ji‘ifi’ZVJ's? ._ , v “#4. A . .‘ ~_; aw?“- ’ . . \‘F ' I}; * ’ '32. “I. ' '1. ‘1 J } .6" I. 'v f r;- {2 -1 9 e‘ c .0 3. (4- f "Jfilud. - ‘5‘. . y~¢¢ --A "n‘. D ‘4’! . 1.x“ ". . . in ~‘5 ‘3. ’3. if 27m 5 ‘ t; .‘ P i .’ O . . , . _ . -u -. , - ‘ . ‘ ' l . Ag _ -a ' ' . *‘ A Q. / . ' . . I ' ' n . 1 . ) , . I ' ‘ r' 3f ‘4' " ,-. r ‘95 k (‘1’. K: ‘ J“I ‘53”. V:- w ! Ir . , . ,,.-..I . "ifiwv" ’;‘.‘. ,. '-~ “ R . 5. {33‘ . _' . : . _ 1 .2 ;, .7}; 21,53; ,. 3w . 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ST: 1L- T 01“ 'l’P‘I‘L'.’ P13. 0 I'LL-L54" The object of this problem is to stucy the uses of activated carbon in the rerovsl of odor and taste profiucing compounds from certain infustrial wastes, particularly, those containing phenol-like compounds. The study is to include a ceterminstion of the quantity of carbon necessary, the extent to which the taste and odor are removed, and the practical application of the process to infiustrisl waste treat- ment. Hentel gives a list of nineteen vaoors and gases that, Hunter, in several articles published 1865 to 1C72, showed snre adsorbed b7 charcoal to a marked extent. Hunter's experiwents covered more groune than those of anyone else at the time. The use of poison gas curing the World We brought back into use the vegezutle chsrs, largely because they had s greater adsorptive cuprcitv than bone Cher. It also s urtee s vast amount of research work on the adsorptive powers of the active Caracas and sethods for proeucing the most active materials. Qhe work of Chaney, Fey and St. John on the preser- stion of active cartons, and miller and his co- workers on the characteristics of the active carbons, has done much to extend their use into various fields of gas adsorption and assorption from solution. lbs activation of carbon requires careful heat control one s usually done in closed retorts. lhe activation must be done in the absence of hydro- carbons or other strongly absorbed corpounos. The hydrocarbons are recovored by cereful s justment of the feupervture and the concentration of the oxidis- ing material. nir, steam one 602 uno chlorine have been used for the oxidirinr mtterisl. Storm active- .3 i. ILiLfl’i'JhY 01‘ ;L(;iI.\/.~...ELL‘ Ciaiilflfii The extensive use of bone char and active carbon in the sugar industry for removing color, and their use es an absorbing material in gas masks, give us an abundance of information on the charact- eristics of such materials. ihe active carbons, however, have been used so little in water hurifi- cation that not much is known regarding them from actual experience. bone chsr, she perhaps some of the vegetable chars have been used to a limited extent in household n.e other small filters for a number of years. Charcoal has remarkable adsorptive sewers. Ftrschen says it seems to h:ve been known that it could be useu for removing coloring mutter from solutions in the fifteenth centurv. He also States that accoroing to Lippmnn wood char Wes utilized about l79h in an English refinerv for purifying sugar solutions. Peter and John Hertineeu patented in hnglsnu the use of bone char in 1515, one this kepfithe use of vegetable Cartons in the background a for several yeers. In fact it was not until gas masks were required in the Aorlo ear that vegetable carbons came into extensive use. tion seems to be rcgeroed as being better than sir. host authors give a temperature of 900 to $50 degrees can rigrsde as tth which procuces the most active carton. ihis, however, depends somewhat on the ease with which the hydrocarbons are driven off. The hydro- Csrhons are slightly less resistant to oxieution then the active carbon. Buylis explains the activity of cerhon in the following way; "Carson as we know hes L valency of four and every atom of czrbon on the surface has at least one free valency. WitL the irregular shape of the amorphous particlcs some of the surface stems may have ‘wo ene occessiocelly three free velencies. ihese free velercies have the power of uniting with or at least 3 erecting to their surface certain compounds that come in contact with or near them." Work on use of aetinteo carbon so fur has been confinee to rtmovel of phenolic compounds and the ci-chlorination of water. That they will re- move ull such taste hroéucing compounds is not likely but it is evieent that they will remove other tests procucing compounCS which veneer in water. nosorption of phenols by the active onurcosls prohthlv has benn known for some life but it was not until the oubliCetion of unsorprion curves by Freunolich in 1926 that it b came widely known. In iece*ber 1W2? Chicago exocriencee in its water supnly the greatest phenolic occurence of any large city in the country. With the “one of neveloning a treatment that woule be less subject to frilure, experiments on the use of activeroo carbon for re- moving or preventing taste one oeor were started in June,l928o The first laboratory filter was mane of 27 inches of eqn:l ?LT*S of Csrco on; bone char. ”star was pollutefi with waste liquor from n br- profiuct coke oven plnnt. The phenol content of the liquor was determined :nd the 'ronortiontl enounts noted to the Lake Kichigen Waters to give desired phenol concentration. In addition to the nhenols there were other cornounfls in the waste liquor that were resovee by the carbon. ihe filter was not run continually but when water was passed through at the rate of two gallons per square foot per minute about fifty liters would he passes through in six and a half hours. increas- ing amounts of ohenol w re added and none or only a trace passefi through the bed until the amount was increased to 100 p. p. m. It was also noted that it we; not until 10 r. p. m. of ohenol was being added that a faint ‘e *e was provuced rfter the scfiition of chlorine, and even then the taste was so slight that it could not be cefinitelv stateo that it was s chloronhenol taste. If the theory of adsorption is correct, complete removal of phenol is not accomplishes. lhere is consiocrable afisorption before enough phenol will rrmsin in so ution to cause a chloroohenol taste. It is not believcc that .001 p. D. m. of phenol can be mane to prewuce a taste, and so long as that enount is not exc coed there should never be e taste protuces by the phenol alone. Kore phenol is actually adsorbed in a filter bet when higher concentrations of phenol are used. Tlis is prohthlv due to the crrbon in the upper bed part of the/sasorhing consixwrebly more phenol than the lowcr part; that is, the phenol con- centration divinishes as the water passes through the bed and the GgullltPilm where the water con- tains consitereble phenol is much higher. This mekes such materials partiCUlsrly sototed for hanIing occasional high p enol occurrences which is the way phenol generally occurs. n Very good adventege of an active ed carbon filtrr bee is that a chemist is not needed to be on outy to find out when pollution starts and ends. As soon as pollution strrts the bed is taking out phenols. The usuel method of applying fiCtiVEtGd carbon is by meens of a suitable dry feed mech- ine equipped with a water ecuctor which sucks in the Carbon enu delivers the suspension to the point of application. lhe volune of wetrr is of no importance; it is merely the means of insur- ing effective distribution of carbon through the wet r to be treated, as the powdered carbon mixes readily with he water to produce and effective suspension. as soon as it becoves wet tnd the pores of the cerbon thoroughly filled with the water in which it is held in susnension it Can be transported :ny distance Cesired without her ing it's ebsorntive prooerties. “noth(r mcens is to Hod it to the rlum either dry or in solution. If sneed to the sclution tank, agitation must be provlued mur- inc the perlovs of use in order to make u thor- ough distritu*ion. lhe ususl point of up lieetion of the pew— cored esrhon suseension is to the water leaving the distribution chanhcrs the flowing to the co- aguli‘ion basins, where the CthO” has e good con- tht period she sefltles out in the h sin to some exttnt. “ha sluCge carbon mixture noes not show the ten ency to putrifeetion exhibitee by ordinary slucgo one conswguently eeriods between busin cleanings can be materially increased. Sore clents use split trebtment evolving part of the Carbon to raw wetcr to stabilize the sluwge that se*tles out. The remainder to the water in the settling basins end is filtered out on the filters, therely increasing their effi- ciiency. AT’PLIC:.‘1’ICT€ CF .AC{I‘Jfld‘xail C; i‘7‘.i;’-'.')I"§ Ii '72." in t3UT“‘-‘Ll.*.if.3 Turing 1950-1951 exceriments were conducted at the waterway purification slant at Fehwny, New Jersey by mortimor Gibbons on the efrcctiveness of Lctivetcd Carbon in removing objectionable odors. It has been effective on vegrteble odors but is difficult to wash out of the filters. Both granular and culverizeo crrhon hvve been used. The rasults genertllv indiorto th:t the meterisl is selGCZivo in its action, being mos? effective ageinst necicinsl ocors. ”he effect of cow cred aciiVnteu c:rb0n on sane filters is worthy of consideration. Filter runs h:ve not been ennreciehly shortened except when large doses of csrhon, more than 5 p. p. m., 0‘ have een used. At such times filter runs have been rreuced as much es 50%. The crrhon is not completely washed out of the sand with the Wash ester velocity of EA inches per minute. i. F. lunger wrote of the use of activated czrhon LE homnort News, Virginia. On account of low enter The water sunplv was t:ken by low in- takes from the rrsorvoirs. {he werrr firs EeVoid of oxvgr_ an. Carbon wzs applier from s Coon Cola barrel that bra an electric bend dr1]_1 with saddles as an n51 ' t.or. CLrbon is inso1uub1e and is faken out at the 11 Ltc rs which mukes it u very flesireahle fuc'or in 1:1 sat-m. n~1.. F. H. Turing, Chief Engineer of fine Ohio Tessrtxgn? of «e'lwfi writes of sci:ivutel carbon. It'h:s been known rhut c:rbou in a si ole form like C‘r‘zesr 0719.11- Doss‘wssvr‘ 119011.111rr Iff.1-V‘Ii’-.'-f~,” for z..‘.‘>:.:<)r1:-ing 1:1.n“1‘:»:in .-"I.s:.onz=:s and 11131211“: fora-31171 sub- ste..1101..s '92-:1. 312311; in 1.1 fluio. 1.c=f.i".:=~.f'.era ChT‘i'Dil is the form npolied to errhon th:t has been proovssefi to rnnfier it rare khan usurllv active in its ud- so rr1tiv Is power. 0 s rcial equip1zmvnr is necfied, 011le 1... (Er-3r .f‘e-' 1‘1 machine 121an watt- r er’ium'nr. “oints of :pp11Cntion vary. rev nafier, n1y1ng a_ha b'mr with chemicals, cosgulsti n basins, or irf1.uent ‘ Ler just prior to flitrxfiion. at New Csstle, Pennsylvania in 1950 the re» moval of fins‘h anfi ofior f1or the water suoplv bee me an unusual problem. a 1ulnt musty to ‘ I ' ‘ 1“ ' ' ’ . ”- -.' - ‘\ .1: o -_- .3 some; 1Lste spectrem in Lao fsr he of fihe Lis- 1 tribution system, not oefec so in the plank. Tncrczsing fhe chlorine (oss stopoec complaints for a while but as the to oersfuro lowerec,the eXoCSsive chlorine Cosc cggrsVutoC rather rhen hel so conditions. 5 ratio of one part of W” to four of five psrts of chlorine gave good results but the £35 treztment just concealed frstes at the plant :no failed 1o control sffier Vestes in the Cistribution system. 13»); l‘c-cez'nlrm 1931 it was apparent that sorts othcr tv‘oe of treatment WLS necesssry. :1 sample of sotiV1tcfl carbon known 99 Euchar was obtained for laborsrorv tests. Jar tcifs contsining 0.5 grains per gallon of notivs196 carbon showed cocplete removal of all tssfie and odor. Aftcr *rying oiffercnt ooints of apolicstion good re- sults were obtained. lo centrol chlorophenol tastes Louis E. Harrison at Bay City convertoo +u0 ssno filters into csibon units, Uyfiro-Isrco is used with the flow fiownwsro. lhe resulfis kre considered quite Satisfactory. Yr. Furrison woes not soorove of the dry feeo mafihofi, although he uses it when the taste in the Wzter supply is bad. He says that if carbon is used in large doses it gives a sulfur taste to the watcr and to get he best results 5 carbon filtrr should be used. Probably the most difficult raw wnt¢r in the United States for trcctmont is at Saginaw, vichigen, because of a very bad trade waste, as well as algae one sewage nollution. it this plant a split terthnt of powficreo actithed Carbon has been USuC’ port of it going to the mixing basin where it sets to stabilize the slufige, the Other part being applied at the secimentetion basins, just before the ester goes to the filters, whereby the cumulative effect of the carbon collecting on the filters is made use of. ibis treatment has reduced the ban taste snc ocor but nos not done away with it altogether. I. ‘9 ..i .f v. -""'IT.' ," . ”ad-"'2 -'I\" .L‘JJ\'1 LILI.‘V.L¢A\ 1-4L fi-kjltl tolutions of phenol-like compounds namely: d’-ch10ronhenol, phenol, ortho éiuchloronhenol, end cresol were prenared. lhe odor value of each of the above solu- tions we 1. “I 8 found 51 the following proceflure. Boil uzguxmdty of cistllumixuMmr until free from omcr emu cool to room temperature. Clean six or more 500 ml. Erlenmeyer flasks ugd remove the last traces of odor by boll- lug water in them for 5 minutes. Iiscard the water unfi coal the flasks, covering them with watch filasses. Letcrmlne the approximate gear as follows: a. Place 100 ml. of odor~ffee KILGT in each of two flasks. b. Term to 70 C. nnfi adfl to one flwsk 5 ml. of the Staple. 0. Shake both fleets vigorouelv, uncover and determine whether or not the water in the flask receiving the sample NLS an Ouor when cwmered wits :hat in the fl- Sko d. If the oflor is oresent, repent using a smallcfl‘:wdtole. e. If sot present, aco more of Jhe sample to the water in the flask until the odor is present. Knowing the approximate ofior, a more ac- \n o curate deforminstion is msoe as follows: a. de 100 m1. of tho ouor-froe n'ter to each of the SGV(Fb1 fltsks. C” Cover with watch glasso» and warm to 70 C. c. To the first ive flasks {do increasing volumes of the sample, takinr Value Ceterminefi to the approximate method. For exam lo, if the 060? wos founo with 5 m1. of the sample in the uporoxlmate metooj, afid 5, h, 5, 6, and 7 ml. respectively to the five flasks. 0. Shake vigorously out determine the flLSk in which the odor first sooe rs. ml. of odor free water m1. of somole odor value ml. of SiWDlG The taste value of the so utions was found by diluting than und finding the value in p. o. m. where the taste coulo vars faintly be fiistln- ‘- guisncd. those coterminetions wore otrried out '- uith taste-free Mata? grepnreu by boiling until free from taste. Various ewounts of activated carbon, known as muonsr, were weigneo out ens Kept in suspension an for a detention period of LU minutes in liter 35391 G, U. of euCh of the orepirefi solutions. The solutions were then filtered and taste mace to in.» b" it} I}. '3 V b. “ all the taste and odor had been removed. fine ooor tests ware mode by heutinr the _) filtrot (D to 70 C. and finding out whether any ooor was still left. lhe taste determlnstion was made b: testing the filtrate one Comparing it with taste-free water to see if any LLsLe I'2-.::.'1L.iilcco {hose yrocooures Hclfi3lfidflfl:tco until the amount of carbon one found Lhtt would remove all {'1’ of the taste ans odor from water so oollu ed. LLP; 1&3 FRSULTE Comgouno Ltor Taste Concen- Grams not. Factor Factor tretion Corbon pogo‘ma __ 7W ri-chlovo- phenol 5h.5 .001 1 p.p.m. .11 phenOl 500 0005 1 poporflo .05 Ortho di- chloro-berznl 21.0 .001 1 p.p.m. .12h Croeol 11.0 .oae 1 p.o.m. .115u One liter samples were used in each of the above determinations. . o CC)n‘.;tn_-_~,1m,<‘-. Cme r'w- C tel-gr; 9'1 {2; t 621‘ 1'08 . Carbon *TI‘ILtIOD Htfiio pom-go Li-ohloro~ phenol l p.p.w. .GCOll 952.87 P118110]. 1 £709.31. .00an 252.18 Ortho d1- chloro-henzol 1 p.p.m. .00012u 1356.90 cr9801 l p.p.m. oOOOllSh 1187050 The cost of Rucher is five cents a pound. From the or :ccding rcsul pin .3 it woalo seem to be Very expensive #0 rerove taste and odor due to phenolic compounos by the use of activated carbon. There is not, however, a concentrytion such es 1 p.p.m. of ohenols in any water euyply. There is no ;'alleble as to her much the average amount of ph n01 in polluted WutCPS is. To prepare a cost table .05 p.p.m. has been selected a" for toe chrege plant. a Fish enough value to take C am; 01 2nd Li-chloro» phenol Phenol Crtbo~di~ chloro—beryol Cresol Concen~ oration 005 pg: 07”. .35 p.o.u. 0C5 pop-mo .05 p.o.m. Cost p.m.g. i N O 0 ex o« \N \N 3-39 2-97 ctivscefi cer“1n will remove the test and odor of ptenol-like cempounos from water. the dry feen metooe of using actiVuted exrbon is ecouowicel only when there is small amounts of phenols in the water sueoly because large ewounts of c rbon will clog the filters arm LeJxa'lt necessrry to wastwtfiwwn.fre1uently3 The Carbon filter befl seems to be the best arrangement for tte ramnvol of tastes and oflors from utter sueplics. inc Carbon aster ratio 0 is must higher 5nd thus will Cause mu h higher remove] at times of ?csty oollutlon. The Carbon filter is easy to control. It is not necessnry for s chemist to he on cutv all the tit-Te as in the case of fir} feed to c‘utrmge the dosage at tl'es of st:rt5ng and stooning of pollution txxemamr- when pollution starts the filtcr is alrezdy asserting the phenols. It is safe to Staff tor-t z:=.(:"lve carbon in water treatment has come to stay, and that its use will increase repielv. 1. 5. 4.1.. 7. 8. J. E. Beylis, "She cc 1Vateé cerbons and their use in reweving objectionable fasfes uno odors." J. hWCT. W.T. L880. 21, 787 (1929) Louis B. Harrison. "50‘1Vetefi Carbon at Buy City's fil+ret1on plant." J. amer. ”.?. r9800. 25, 1538 (1951) Eelcolm Pirnie. "Exnerience with powdered activated Carbon." J. LKCP. W.T. $5800. 25, 1595 (1951) E. 3. FurMLn. "Pemedving tan+es and ofior conpluints resulting from water supoly at To'edo." ‘V.‘T. not. 85, ERG (1Q32) n " Paul thSLE. "]_scussion of papers on actiVated urbon." J. nmcr. T. T. :98000 2?. 1&6? (1950) I! a Charles E. rowbrifige. Letivnteo oer on re- :0 ‘f' F) (‘f C) (D moV9‘ mud Doors ffiom weter. Dublin “OVks f2 *0. 6, 19 (1051) E. A. gthnS. Tysfe elimination wifh now- Tetfr Works and rewcrage 789 11 (1751) h . H, L ' -. I! _ n . F. lugger. "cos 9 eon 000? removal. ”atcr Works and Lewersge 78, 378 (1951) 9.J. h. Buylis. "3%e .ere for reference Labor- tory for activnfcfi orrFon ”. W. ané Few. 10. 11. P) J». 13. George h. Lpuloing. "notIVetec char as e 4 deodorant in water purificxtlon." A. d. Eehrxen éflt H. 5. Crane. "Chemical and mechanical utilization of ecfiivated carbon in water purification." J. an. ". *. assoc. 22, 1399 (1950) J. F. :uylis. "Further ovservetions on the use of activated carbon in removing objection- able tasfies ant odors from water." J. 5m. V. W. A3900. 2?, 1&38 (1930) G. K. Eorcom and h. I. load. "Lafiivuted Carbon for *he removel of taefe and oflor." Jo If”. ”‘0 11". #30000 229 114—1“- (1950) I—__—AA-—-- - 3_ ‘ -'l.-_ 3‘ -4 A h F ”"TWWWV ' ." . . '1r 4d anggwu EQ51V LPrr"r 1111111111111 142 6517