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W. .2". e «as... . ;.. ‘V 13:33“ .v3r A STUDY OF THE DISPOSAL OF CREAMERY WASTES A THEéis,SUBMITTED _To THE FACULTY OF THE MICHIGAN STSTE COLLEGE *'3(-* BY C. E. SLAUGHTER CANDIDATE FOR THE DEGREE OF MASTER OF SCIENCE June 1926 TH E515 TABLE OF CONTENTS Introduction;/ Legislation Present Status of the Problem Conditions governing tests ‘Methods of Making Chem. and Bact. Tests. Inspection East Saygatuck Pearl Creamery Hartford Creamery International Milk Prod. Co.,Bad Axe. Caro M. S. C. Dairy, Tests Questionnaires Constituents of Creamery Waste Disposal Methods Dilution Storage Septic tanks Contact Bed. Storage with fixed H. GoncConc. applied to Septic tank Chemical precipitation Travis Process General EXperiments. 103773 - 19 19, 20 20-23 24,25 25 25 26~29 29-33 33-36 36—42 42-45 46- 47,49 49-56 Chemical Precipitation, Cont. Relation between Acidity, H. Ion Conc., rate of settling and color. 56—58 Effect of Chem. Precipitation on Bacterial Flora. 62 Septic Tank Principle and Chem. Precipitation 63 Results obtained when Chem. Precipitation is properly carried out 65-67 Sludge 67 Conclusions from Chem. Ppt. Exp. 67 Recomendations for design of disposal plant using Chem Ppt. and Sec. Treatment 68-70 Cost of Operation 71 Advantages which Accrue from the use of this system 72 Suggestions for future research in this subject. 72-73 Summarsuoflaeonclusions 74 Refferences 75. Fig. aims-Cums: 10 11 12 13 14 15 16 17 18 19 2O 21 LIST OF ILLUSTRATIONS Discharge from E. Saugatuck Creamery. Seeping Cesspool used at Hartford Creamery Disposal Plant Arrangement at Bad Axe. Automatic device for dosingprecipitating conpound Dosing Chamber at Bad Axe. Septic Cylinder for studying effect of storage on 2% Milk Waste. . Chart showing effect of Storage on Oxygen consumed and acidity of 2% Milk Waste. EXperimental Septic tank and Contact Bed. Chart showing Acid formatiom.at various H. Ion Concentrations Chart showing decrease in Oxy Cone. with Fixed H. Ion Conc. Illustration showingeffect of Chem. Precipitation Showing results of Chemical precipitation Same as Fig. 12 after standing 14 Hrs. Same as 12 after 32 Hrs. Chart showing effect of various quantities of Ferrous Sulphate on total solids Color Chart showing change in color and appearmie of Ppt. Corresponding to Various H. Ion Conc. Showing effect of variations in Ppt. proceedure. Showing change in Sludge in Fig. 17 after 3 days. Various Effluents Diagram of fixed pH. Septic tank Suggested Arrangement for Disposal Plant. ACKNOWLEDGEMENT It would be impossible to individually acknowledge all the aid that has been extended in writing this thesis? However, great acknowledgement is due Prof. Mallmann who gave no end of aid in its development. INTROD{_TC TIL Cl: average creams ry the importance of this subject will u; apparent. erclvc’ fr‘: 1*.2rnat‘"" nilk Tnztes. Th1 is the n '1 . o‘jstf' n =—;* m..‘“r 'xersg: erSon but there are other ‘ 11-94” :- L ~2. ’- " ‘._ _..,."'. '\l.|..3‘:ab::. '--vr—‘ 1‘; Ch 3Tb not SO 1 ‘ generally *ealizei. It has been found that milk; wastes not only have 5 toxic :ffeot on fish and other aquatic life but als cause their death by suffocation by sfiosorbi ng . . the :1-- 1-fi4 -~~~nn q - J‘njflr rfiub=n ann41+4 pa 4 _ = u... 70_\/"..- anvil. . {1'}- ‘QI‘C' ALI-v ”:9 DILKV Lu \. ‘........u...l')--o Ln I a stream.* . 1, _-L ..A_.. . ..,~,...1.I 1...... ‘-,~ .. . tendency tflnh the s.rea; might 14v: .:d is relinei and a .1. z 1 , 11. - ,- L menace to p121-” . b.- (A..U$. . 1 11'. .n I. -. A. +- 1... ....4., . ,,. is....icn o. 3.13HW. .J .ra.. u.wc s and more (D U1 0 (D D D—k f-‘J .J H K: {:1 r) roamcry wastezz .- .Lcrefore a serious public Such pollution also has an o..ononic :ign1ficanse Our stroc.:s and Take: Nat“ their scenic effect and the .....1 ..n--4.. -. an a....;. .. rocrczt.c saw niniin; ...y a..ord constitute . oat ’ natural resource my irsw:ng to Eichi; “a1 vast numbers of . -_ . m .. . .. - . .. - ' .1-.- . A. n tOdria s uh, every year a an? in the neighboflva I.” ‘- .. - . r .. '. .... -"!-~‘!- t'entJ-tELet lien 1t.l.rs'. * Cornell Universith Exp. Sta. Pulletin, u ’s;)osa.l of Dairy WHstes, p 61 ** Mich. State _.o.servation Dept. Estimate. The which in tTr ‘rfi: has presented a problem since the .beginning of industry, and hasAbecome more serious as. the Li‘s-fir: star: i'cr‘""--=.,.'-.r':--‘: 2-”. -'.'n..--::1f_.':_t:.', has resulted in some important le:.siation which promises t: become quite an issue wit“ those Jidnctrie: Jhesc wastes are difficult to lisucsc cf. In th early history of the State the bad effects f certain wastes were realized. This in 1?65 we find in, Art 350, 13 3, an Act to Protect Fish and Preserve the Fisheries any of the wat;rs of this State, where fis any offal, blood, putrid brine, or filth of any description and any person so offending shall so fined in any sum.not exceeding $300 or imprisonment not exceedin= )0 da"s or both at the discretion of the court." "Provividfitbwever, that this act shall not be construed to apply to discharging the waste matter of “J any paper gill into an (a: C} the streams or their tributaries :34 F0 on sections 13, 23, an. 4 of Schoolcraft Township, Kalamazoo County." Although this act prevented gross pollution, in many instances, still its ineffectiveness is seen in the deplorable condition of many of out streams today. The paper mills around Kalamazoo were exempt from thee act, probably, for the very good reason that \absolutely no method was availabee for the diSposal of l . their waste, and these plants are still discharging , their raw wastes into the Kalamazoo River for exactly the same reason. ‘ The act that created the Conservation Department in 1921 also placed the responsibility of pollution prevention- in their hahds, thus, Act No. 17, 1921,5ect. 3. it is to be made the duty of the Department of 'ccnservation to protect ani conserve the natural resources of the State of Hichigan,w-~-c--~—c— to guard against the pollution of lakes and streams Within the State and to foster and encourage the protection and propagation of game and fish." Some beneficial results followed the creation of the Conserve ion Department. However cosy felt the limitation of their authorit*. Many creameries and—ether— factories continued to discharge their wastes into the streams in tkcwfieee of restraining orders from the Conservation Department. Hence the Act of 1925. Act No. 201, 1925 "Section 3 of Act No; 17 of the Public Acts of 1 .. , H 1921 is nereby amended to read as follows. "It is hereby nadc the duty of the Department of Conservation to protect and conserve the natural resources of the State of Hichigan and°~~v«——---~---~- to guard against the pollution of lakes and streams Within the State and to enforce all laws provided.for that purpose with all athority g anted by law and to fostei an; encourage the protection and prepogation of game and fish". By this act the matter is placed squarely before the Conservation Department which is now vested with full power to enforce their orders. PRESENT STATUS OF PROBLEM On March 50, 1926 a hearing was held at the State Office Building by represehtatives of the Attorney General's office , ' . of'Health, and Conservation Departnent. Representatives of all the important creameries in the State were present. The future policy of the State was outlined. in l a general way and it was announced that the creameries would be given thirty days in which to formulate a plan or a program leading to the satisfactory disposal of the wastes at their reSpective plants. v—3 :5“ (D L) C in -tc Departments, very properly, steadfastly refused to set any standards for treatment or to recommend any process. The problem of finding a process which will 'reduce wastes to a stable effluent is left entirely to w the creameries. 3 The creamcries are now facing the lilemma of L) i ', ., _ ,2 ,. ~\,,. , q. A...a. -. 1 ' immediately alanllnr nwufi lispooal Sys em fur wastes ) when th- Baird of Tcalti freely admits that no reliable 'T v_——4 \ \ What little resecrch has been done in this field has been mostly in connection with fairly large inflexible tanks] fed by createrics Th-se wastes vary greatly in volume, quality, and concentration from dry to i5". In most cases the design of these paants did not lent itsel- well to e'-:rim inflet'hility their . Such large so valuatle; In fact nece factors :nter int» the s 4. n - ..U ”9,8 “9;? ', proceeded hr 3 J ,“/, \rd‘.(f'—yfi ‘.,L. I ‘ (- 9-4.: n. .1 .. . 1. ,. o ’1 Ya , r~ r' DOL1.e .Llln ldAiA'enlJ(..1 'inLJ 1 mx’l: ,— -l-‘—\A 9. ' ~ ,_ WA ‘ ..,‘L .Li L»; n.1,,” .. x; JJ" ”:Q(3-lb 57 ..n19+1 a k, .. 1’_)rK,_L ii (.3 4—, -', . . L‘,‘ A 1 4" ~ 4-. 2-- [J/jJ—E‘.) f3”- .} hi. )‘:'J» O u $‘n ~" - n I‘D" " I" d an q‘“ 1-6.11.1 iii ‘1‘ w , . ", ,3 .-" 'n ”,4- ~51 1-, r H an '_ S‘) (J I‘IV lg: . JL' ‘1 [L3 . 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'V «2‘ - ~.- ‘- 1' — 4 ‘a A 3 r- .a A. r . x t If C"? 1:1",fftw‘f2r'. J7 AI‘J' ,U. COL") "\IT‘ 'I :3 .4 -.‘n ffi.‘ 6"? -:'S OS, - 4- P ‘- x ., , m ’ 4- 4 3. , 'fi '5 ,1 + p w-r 1 4-‘a mo". C- tau Jo+r. .B!s fifionk -2 .fiuenoe' do lo flto o;o n k a “, " ‘ 1" ' D 4"» VI' " f' X" *7 "’7 I“ 1 1‘ 2 ~+ l‘ ’3 L‘.apLJ-t .1702" ."' t 703+; Oi “A ‘ n");:»L,€;;§ LL\1 v c1” 1C0 ’7 c1 aiEJLJuLALC‘C; f ”SIR/9 1A**v\r TC“: F.” to I'- stajnute rozuiffTS iv o odors imaginakln, A fifo outlet is skown “n “53. ”he orenvprv P rxyn t‘xE Cfl’udhi.f;' "n” use a iiffflanf :oiVUT ‘0 1‘ -- 1-1“ ( f3 ‘ A -v . .v- .s , v fine. ‘fi'khfill’ 3003 uuaJ uni -Lm1\$\’: y‘fl'.‘.l\ r 1 L1, ~ Ayfi- :I‘“"‘l LL KL(.:\41JI\‘11 ; L '10 “LU-‘3": Clad)" -.k.'L, :— ..h w , 9 L , . ,. ,. , 1 A , ° mfh ”1 ;fi€ 31.0u an»? fan iriin 1 J o -, - . _ -1 v ...1. .g reco.vefi numerous comm. 1Los .~ n ..x 1 % -..». ill - ’2 lC‘uuLCdij ».€ 1,1-.115‘13 V711 t0 ,2 . ‘flv-“-~‘ .1 L\ 1 Q P .'.j,gn. defore ;ong. 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The new tank,Fig. 2 was rapidly filling up at the date of inspection and it seems probable that it will be necessary to clean out and relocate the tank once a year or oftener. International Milk Products 00., Bad Axe, Michigan This plant was visited later in the fall, October 21 - 24. It is located in the outskirts of Bad Axe and its business extends throughout the thumb district. The plant uses 50,000 to 65,000 gallons of milk per day and manufactures varying quantities of butter, condensed milk, milk powder, etc. Mr. Gibson, the superintendent of the plant, stated that the quantity of their wastes varied somewhat but amounted to approximately 325 lbs. of solids per day. Until last year all of the whey and other by-producss of the creamery were dumped into the disposal plant which was designed only for municipal use and Bad Axe was widely known for its disposal problem. Unless the wind was blowing in the opposite direction the entire city was pervaded with odors from the overtaxed disposal plant. At present the creamery separates the whey and more concentrated milk- wastes and hauls them to a distant orchard where they are dumped on the surface of the ground, and used for what fertilizing value they have. The wastes now consist of the 325 pounds of solid matter, enormously diluted with 13. _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ n _ u M _ _ .5\V\_\ .x..\ n _ \utuuhz u n _ _ u _ _ _ _ _ _ _ _ _ _ _ _ m _ / . z _ / _ / _ IIIIIII ._ /" {#wa _ I. lllllll I \thh/ _ task I at} $.th 5.13:6 lllllll L was: . .. - aim _ \xs ... ”Min.“ : I I \‘k .‘N\90D‘OH\H~*¥§QE§*3§ \‘NQQ EN! Musx 8R —v .kIMMV m. . I I I II I l i_ the _ llllll LL 18.0 _ S\v\.“\\\5\§< XWXV Q‘Q lllllll I. ks<<flnk NVW§KM.Rem0't ions“ . ("fp/ Relative stability of effluent Oct. 29 20% Oct 30 4% Nov.10 8% The relative stability seemed to bear more relation to the turbidity of the Sample than to the amount of organic matter or the period of storage.y (“The inconsistent and abnormally low results‘ were probably due to the absorption of the methylene blue dye by the colloidal and suspended matter.* , I Conclusions from Operation of Contact bed. (1) Using a retention period of thirty minutes W1?“ a reduction in the oxygen consumed of 7% newbie easy * Taylor's Chemistry of Colloids. 6¢'\n.,\b& . it)“: 36 . expected. This-W121 be accompanied by a rise of about 7 % in acidity. , , (2) The relative stability tesy.iepnec applicable to effluents of this kind. (3) The operation of a contact bed for this purpose result; in very offensive odors. (4) It would seem, therefore, that contact beds are not satisfactory for creamery waste disposal. FIXED HYDROGEN ION CONCENTRATION Since septic action had failed because of the rapidly rising acidity and treatment in a contact bed had failed to produce any further material reduction, it was thought that by preventing the rapid rise in acidity the bacterial action might be continued { Accordingly a series of five four-liter glass jars were filled with 2% milk solution and by the addition of calcium hydroxide were brought to hydrogen ion concentrations of pH 7.6, 7.2. 6.8, 6,4, and 6.0 Once a day enough calcium hydroxide was added to bring the pH value back to the previously determined amount. Some interesting observations on the rate of acid formation were made, Fig. 3, pfiifl. The ordinated- are the pH valueyfia;which the waste had elfijheg each day before being neutralized with the calcium hydroxide.' It will be seen that most of the acid production took place during the first two or three days. The great 3‘7. 4.8 c570 £2 to & .... . § can §\\{V\a\\.\ a J . 1 c ( ‘wki asfik.§\\\\.\\\ t\ ¥S\\\\N , _ 38. improvement of this method over ordinary storage can be a seen by comparing this diagram with Fig. % where acid formation continued for several months. Since the rate of acid formation indicates the rate at which lactose is fermented the great advantage of keeping the waste alkaline is obvious. The data that was obtained from this eXperiment is contained in the following table. Fresh 2% milk solution ---Solids -------- # pH Oxy.Cons. pH after 24 Hrs. Total Grease Ash Org. 1 7.6 1065 6.8 3480 750 350 3130 2 7.2 1065 6.6 3 6.8 1065 6.8 4 6.4 1065 6.4 5 6.0 1065 6.0 First Day -------- Solids---——---—-- pH pH after 24 Hrs. Total- Grease Ash Organic 7.6 5.4 2710 430 350 2360 7.2 5.8 2640 270 2370 6.4 6.1 # 1 2 3 6.8 6.0+ 4 5 6.0 6.0 Second day \n n- \u m H at pH 7.6 7.2 6.8 6.4 6.0 'pH after 24 Hrs. 6.4 6.4 6.2 6.0 6.0 FBurth‘Day Ln c— \N m k‘ we pH 7.6 7.2 6.8 6.4 6.0 pH after 24 Hrs. 7.2 6.9 6.4 6.0 5.9 Fifth Day \n c— \N N H 4: pH 7.6 7.2 6.8 6.4 6.0 pH after 24 Hrs 7.3 7.0 6.4 6.3 5.9 Oxy. Cons. 660, 659 605 650 650 710 Oxy. Cons. 510 Oxy. Gone. 430 455 468 429, 434 494 Seventh Day # IpH pH after 24 Hrs. Total 1 7.6 7.4 3820 2 7.2 7.1 4200 3 6.8 6.4 4 6.4 6.2 5 6.0 6.1 # SuSpended Solids Suspended ' inorganic l 1872 296 2 948 136 3 82 8 116 4 5 800 38 Eighth day # 1 2 3 z, 5 40. --------- Solids-----—----—-- pH pH after 24 Hrs. 7.6 7.5. 7.4 7.2 7.1 6.8 6.8 6.4 6.0 6.0 grease ash organic 140 2430 1390 1030 2170 Oxy. Cons. Filtrate 21 12 79 105 mc/ any. (can: t. c c Ruhr for Mil/Ill. 2 «3' 1 lo Da/a' —— Sines]: . ‘7‘- Fig. I?! ‘ 5 Fig.§$ shows the decrease in oxygen consumed that occurs when 2% milk solution is stored at a constant is shortened up to about one—tenth the time required with ordinary storage. 9. Fig. I it will be seen that the process of reduction 41 hydrogen ion concentration of pH 7.6. If compared with It was found, as shown in the preceeding tables 6’38§?39i 40. that at the end of seven days most of Kr" the solid matter is in suspension and that after this suspended matter is removed by filtration the oxygen consumed is very low, 21 p.p.m. when stored at 7.6 pH and 12 when stored at pH 7.2 If it had not been necessary to mix the waste daily in order to neutralize the acid and if the 42. operation had been caried on in a larger tank a much better effluent would probabpy have been secured because of the better opportunity for. sedimentation. (One important feature of this prosess is that N offensive odors are greatly reduced. Septic Tank Action with Constant Hydrogen Ion Concentration Although the bacterial action was rather slow in Pi}: 3' ' I' ad in the preceeding experiment it was eXpected that when the fixed hydrogen ion concentration principle was applied to a septic tank and a portion of the gigfgzgtents was retained to seed the incomming influent, quicker action would be secured. This proved to be true. Referring to the table an d Fig. Tilt will be seen that pH 7.6 was the most favorable hydrogen ion concentration for rapid reduction of the waste. and it was,therefore, selected as the one to be used in further eXperimentd . A four liter jar was filled with 2% milk solution and inoculated with bacteria from the preceeding eXperiment. Once a day, two—thirds of the liquid was siphoned off and replaced with fresh 2% milk solution. The resulting mixture was then broughtt; to a pH value of 7. 6 This process was continued for about a week 43 in order to stabilize the action, then the following analysis was made. Total solids 2510 Inorganic solids 370 Organic solids 2140 suspended matter 92 Acidity 17 Organic nitrogen 67 Oxygen consumed 362 Oxy. Cons. after suSpended solids were removed 226 Bacteria --------------- Dilution ----------------- ,2! 1/100 1/100091/100,000 1/1,ooo,000 ' NMAmMamNASpPeadePS Total -—-Too thiek- 46,000,000 47,000,000 Acid 7,000,000 Neutral 20,000,000 Alkaline 20,000,000 Casein liquifiers - 3,000,000 In order to determine what would happen if the process was neglected for a day as might occur in an actual plant over a week end or a holiiday,~the change of waste and restoration to pH 7.6 was omittedaOne day and on the next an analysis was made with the following result. Total solids 1930 Grease 0 Inorganic matter 650 4.4. Organic matter 1280 SuSpended solids 460 Organic Nitrogen 72 Oxygen consumed '211 Oxy. Cons. after removal of SuSpended matter 155 Bacteria ----- r ------- Dilution ----------------- 1/100 1/10000 1/100,000 l/lpoo,000 W/wwxr. cruel]! Total Too teach --- 49,600,000 52,000,000 Acid 8,000,000 11,000,000 Neutral 23,000,000 31,000,000 Alkaline 18,600,000 10,000,000 Casein Liquifiers 200,000 1,000,000 The advantages of maintaining a fixed hydrogen ion concentration are evident. It was possible to accomplish far more with a retention period of one day than with three days in the ordinary septic tank. It is probable that with a large tank considerably better results could be 9 ) secured because of the more perfect sedimentation . The effluent from thee process, moreover, is less cloudy, and has a much better appearance than that from an ordinary septic tank. The odors while somewhat offensive are not nearly as bad, The scum and sludge accumulation is not nearly as great and the scum is less offensive. 45 Here again the relative stability test failed because of the cloudy condition of the effluent but the fairly low percentage of suspended solids indicated that the effluent might be safely discharged on a sand filter without danger of rapid clogging and the low acidity would facilitate rapid oxidation. It is also certain that with a longer retention period better results would be obtained. Conclusions from Fixed Hydrogen Ion Concentration Process. (1) The decomposition of milk wastes is greatly facilitated by the addition of proper amounts of lime or other basic material. (2) Best results are obtained when enough lime is added every day, to bring the hydrogen ion concentration to pH 7.6 (3) The effluent, being low in acidity and suSpended solids is suitable for treatment on a sand filter. 44) The sludge and scum accumulation resulting- from this process is less in quantity and less offensive than that from a septic tank. (5) This method of treatment can be applied to any septic tank, thus increasing its efficiency many fold. .CHEMICAL PRECIPITATION Many serious ahyecfic'm were common to the results .of practically all of the laboratory experimentafinnr1fiwedl j (These seemingly inherent features of creamery waste disposal include, the heavy offensive accumulation of scum. the objectionable odors of the effluent due to the decomposition of the large quantity of protein, the large amounts of grease, and the cloudy nature of the effluent. These problems were all met in a series of experiments using chemical precipitation. Chemical p recipitayion as applied to creamery wastes consists of adding the salt of some heavy metal such as ferrous sulphate and precipitating it with a base such as hydrated lime. Fe 3 04 + ca (OH)2 ----- a- Ca 5 04 + Fe(0H)2 The ferrous hydrbxide forms as a heavy gelatinous precipitate which on settling drags down all of the suspended matter. (9.4:. H til-v This method has been tried with lettge success sewn?“ in the disposal of creamery wastes. The opinion is popularly held that this process does not materially reduce the oxygen consumed, that an enormous quantity of ) sludge is produced, that the process is difficult to carry on, requiring considerable technical knowledge, that its ' 47. use inhibits bacterial development, and that a poor quality of effluent is produced.) [Thatwmost of these ideas are fallacious when the process is properly carried on is demonstrated in the following eXperiments. The Travis Process. NSQhasdbecnpmentdbnedubehoes Che disposal plant at Bad Axe is One of the'few plants in the country where chemical precipitation is attempted.) grassed; ni'ch“;;~‘.”rstpes highly diluted and in combination with municipal sewage amount to about 120,000 gallons per day. The precipitating compound used daily consists of 600 pounds of dried marl, 200 pounds of hydrated lime, and 25 pounds of ferrous sulphate. This is equivalent to 0.025 5. of frccous sulphate per liter. The process, a‘Q/[s'armes out at Bad Axe is obviously ineffective but since the plant was somewhat over loaded it was thought advisable to try a few experiments using small quantities of ferrous sulphate at various degrees of alkalinity. The results are shown in the following table..§f&84/The 1% skimmilk solution was arbitrarily chosen because the wastes at Bad Axe are: somewhat more dilute than the average. 48. O. O. O. O. Q. 0. .0 .ccsacppo nuances soon exp ca seem ma pecspccsp mo conpcs mace do mmosm>aeocmmcsa one .csHH odd cpcSQHSm meoaacm Ho mandosc Hanan c>apcaca means mpecsHacexc caom mo nuances one waampsoo manna chops one were . cam ncam comm Ilooam ommam oscm aa.o m mno.om ooam mmam omcw oeem omnflw “momam NH.o m owo.om om mnmm ommm comm oeawm owcm NATO m moowam ...... W anew omeam omam oemam osom oo.o W ooam salad“ .sdém .mdiem .s.m. ...smudyi 6.83m confidence 85on season. season. season. moaaomsseaaomc.nsoo .axom owes -eomcm m acaeaassaem .dmsm“ oooscdmsma eassmao“ .maosHa Hepoaa .mLUsH .csaq can openeHSm crossed mo moapapdtdd Hanan spas condone soapsmOm sadssdxm R H 49. The original Travis process, as used at Bad Axe. failed to give results and, using concentrations as high’as 0.17 g. per liter of ferrous sulphate. no appreciable results were obtained. Unfortunately Mr. Travis failed to answer the correspondence of the writer j;and nothing could be learned of the principles of the i process o_n how it came to be developed. General Experiments. In order to determine roughly what might be expected by using widely varying amounts of ferrous sulphate and degrees of alkaldnity several general experiments were tried. The results in the following table are typical. 2% skimmilk solution Mil. Eq./ L Ferrous Acidity Oxy. Turbidity odor sulphate Cons. after Ca (0H)2 g/L p.p.m.' p.p.m. 3 days. 5 0.1 +190 570 Cloudy ++++ 5 0.4 +580 640 Cloudy ++ 5 7 1.0 -------- ---- Broken ————————————————— 15 0.1 +260 680 Cloudy +++ 15 0.4 +310 570 81. Cl. - 15 1.0 e490 650 Brown - 30 0.1 +40 850 cloudy + 30 0.4 +50 840 51. Cloudy - 30 1.0 +70 810 Clear. - 0 Fresh 2% O 670 Cloudy +++++++ Skimmilk 50. Fig. g3 Chemical precipitation experiment This shows the appearance of the effluent and the sludge that formed when one liter portions were treated as indicated in the preceeding table. No. 3 is missing, having been broken earlier in the experiment. It will be seen in the preceeding experiment that best results were obtained when the acidity of the supernatent liquid was lowest and about 0.4 g/l of ferrous sulphate were used. This was further verified in the following dada We 51s 1 [Here again it was apparent that the clearest effluent with the lowest oxygen consumed capacity was obtained when the effluent was about neutral. In this experiment it was between samples 5 and 6. 51 .noapsHom Mada maons Rm a mo mzoapaom ampfia ode wnamd moss mama mpmop obonm one omm oomm ssoam semao OHm om» oam+ m.m om m oom omom esopm samao om» com owa+ q.H om a o + 0 0mm oommsopm Hm aon0 00» CON om m H om m omH ooompmonmoao hsmHo 0mm o¢oa om: 0.3 om m oom osmH awmao =.Hm 0mm onHH on- m.o om a oma cams =.Hm aesoao oaw cam oe- m.o om n omH ooom aesoao assess 0mm omHH op- ¢.o om m mma comm aesOHo aeasoo oew omoa om- m.o cm H nm< .9 mam ma .saa 0H mama m .a.m.a .s.m.n popaa\mawaw momov mo .02 topoa .msoo apasao< oesnmasm a \.em .Haa anaom madness maoo .axo .axo msoanos 52. «V Fig. la. '1 This picture shows the one liter samples of 2% milk solution treated as indicated in the previous table. This was taken ten minutes after treatment. Note that the sludge has settled very quickly, also that Nos. 5, 6, 7, and 8,which are not excessively alkaline,are clearest. ‘_ m. I ,A ,7 , 8’ Same as Fig. I? after standing 14 hours. The excess Ca(OH)2 in No. 4 has been neutralized by the formation of lactic acid and it has cleared up. Note the dark color of Nos. 6, 7 and 8 due to oxidization of excess ferrous compounds. 53. Fig. fir“ Same as Fig. 335 after standing 32 hours. The acidity of numbers 5, 6, 7, and 8 have risen to such a point that the casein has precipitated It can be seen as a thin white layer on top of the sludge. If the basic material had not been added first the casein would have probably been removed by the precipitation. 54 3000 2600 A040 h A h 1200 )0 IGdO 72fiV'JbfiU0 - Fbrfir// 012 0,4 ’0‘ at? ’10 ['2 ['4 I,‘ Fer/'4 44' Ju/lbédfl' ijMr/Zli‘c'r. Fig. 15. Fig. 15 is a chart showing the effectiveness of the various quantiyies of ferrous sulphate in reducing the amount of total solids in 2% milk solution in the preceeding experiment. It will be seen that 0.6 g. /liter of ferrous sulphate is'the least quantity Which gives good results. L 55 Proper Order of Adding Basic material and Ferrous Sulphate Casein is present in milk in the form of a suspension but it behaves like a fairly strong acid and dissolves on the addition of small amounts of alkali.“ It is obvious that if the basic material is added first the casein will dissolve and escape presipitation as it did in the preceeding experiment. If the ferrous sulphate is added first this will be avoided and two other advantages will also be gained. Ferrous sulphate is the more expensive compound and if added first can be used in the most economical quantities, and the basic material if added last produces a color change which will aid in seduring the proper degree of alkalinity. : {Forbest results the ferrous sulphate should first be dissolved in water, a 10% solution being convenient. The proper amount of this solution should be added to the waste, first. Absolutely uniform distribution is not necessary but some mixing is desirable. The lime or other basic material should also be made into a solution. It should be added slowly with constant niXing in order to avoid a local excess of alkali which is shown in a later experiment to be detrimental. » The. color chart, Fig. 16 will aid in determining té:;proper am_ount of basic material. I ” As far as could be determined equivalent amounts of calcium hydroxide and sodium hydroxide gave identical results and the latter was used in subsequent experiments because of the greater convenience in handling and storage. 56. RELATION BETWEEN ACIDITY,HYDROGEN ION CONCENTRATION, RATE OF SETTLING, AND COLOR. An excess of basic material should not be added. It is not only wasteful but it inhibits bacterial growth and prevents the precipitate from settling readily. ; [fprrecipitation'is complete the amount of ferrous hydroxide dissolved in the uupernatcnt ldquid is more than enough to give sufficient alkalinity to insure good bacterial action. The solubility of ferrous hydroxide in cold water is .0067 g/l * 0.0067 x 2 _ Conc. (H)+ x Conc. mm" = 1 x 10' 14 Assuming complete dissociation at these high dilutions pH= 9.7 In order to study, further, the effect of different degrees of alkalinity on precipitation sucessive_gmouats’amounts of NaOH were added to portions of 2% milk waste and the resulting acidity, hydrogen ion concentration, and behavior of precipitate were noted. «y 57 _TABLE SHOWING THE RELATION BETWEEN ALKALINITY, HYDROGEN ION CONCENTRATION, AND BEHAVIOR AND APPEARANCE OF PRECIPITATE. 3 liter portions of 2% milk. 0.5 g/liter of ferrous sulphate. Color immediate cc. 50% Alkalinity Supernatant Lately after . liquid after treatment, NaOH Normal pH‘ Precipitate precipitation before settlggg 0.00 -0.0l70 6.4 None Light yellow 0.50 e0084 6.9 Very light green Very little light bluish settled out slightly in change green. 10 Id 111‘. ‘ 0.75 10078 7.3 Light blue ppt. Cloudy Very light forms readily greenish blue. settles slowly 1.00 -.0070 7.6 Large light Clear with a Medium Blue. blue flakes of few flakes of Ppt. form almost Ppt. suspended immediately and settle fairly well in 10 Min. 1.25 -.0050 7.8 Med. Blue ppt. Settles out very quickly, leaving‘ Clear Medium Blue a clear Supernatent liquid at end of 10 Min. 1.50 8.0 Medium Blue ppt. Settles out quick 2 _ 1y. Clear Medium Blue 2.00 +.0015 8.0+ Med. Blue ppt. Settles out . quickly. Clear Rather dark blue 2.50 +.0049 Darker ppt. Settles out quickly Clear Rather dark blue. 3.00 +.0052 PPt. rather dark Slightly blue. Does not settle out so readily. cloudy Quite dark blue 58 Table Continued. Supernatant Color immedi- . liquid after ately after cc. 50% Alkalinity precipitationt treatment NaOH Normal pH Precipitate _ begore settlg 4.00 +.0091 Rather dark blue ppt. Does not Cloudy' Quite dark fib settle out blue 6.30 +.0277 readily 6.00 +.-225 Settles out Slowly Cloudy Quite dark 10.00 +.0385 Settles very slowly Very cloudy Dark bluish slate color 14.00 +.0584 —No ppt. No settle— ment Dark It will be noticed from the preceeding table that good precip— itation took place at a H ion concentration range of PH 7.6 to well above. PH. 8.0. This PH range is also the most satisfactory for bacterial action as is shown in Fig..5'&3, In fact it closely approx—l imates the alkalinity of domestic sewage which ranges around PH. 7. Q {The change in color and appearance at this point is quififizégrik- ing. A medium blue color and the formation of a heavy featherylpai. indicates that the proper amount of alkali has been added. If the mixture is too acid it will have a light buff color and lg too alkaline the color will be dark blue and the precipitate will not form. .\ X} e or changes that accomwany Varying degrees;of alkalinity J;' are own in gig/16. L«/” A few experiments were tried to see if the process could be \ 4 ’ \ \_«.' " reversed after too much alkali had been added. I’The sample in the preceeding experiment which had been brought Mctk41¢T to an alkalinity of .0584N, at which point no Q£;, formed, was P,I?9stsd_..wikth essaeseiveamounts..913-w,1_:hsris..acid.— The mixture»! _.._ SHOWING CHANGES IN 004 OR AND HPPA‘A RANC‘E 0F PHEC/P/TATE j " CORRESPoNo/NG 7'0 VA Plat/J HYDRO. 66” MN ico/chr/v TRA T/OIVJ. ] ‘ 3 1 g . J 3 u éngejgfif fly 5.4 P’“ 6.9 /o//,7,3 kfl. Z6 *5/15 Iggy ##834 5“”m’? W/W/Mf/W/ -.'0/70 —.0€84 —. (7075) aggro .., 0050 7550 {J 7‘ .0019 +,o 002 1'— 005/ +ozzs‘ 7‘ . 45295“ 7‘ ,ad—84. Appearance IMMfa/ld/zé/ affcr fi‘f’fierwxca/ Treafme/fl‘i \ fl/u/beara/zrc 7‘22; mum/2‘5: affer CAeM/ra/ (fKC’J/Mt’nf- ,r/y, /6 l weq‘ T 59 ._//;;2\\\ipnt fluough approximately the same color changes but a precipitate ‘5 did not<égmm3npelhg)form until an alkalinty of .0018 orfiébt. 8. O was reached/ Beyondhthis point a precipitate formed but did not settle readily. Some of it rose to the surface and the remaining liquid was cloudy. (sample #1 Fig. égiag/) 'Another portion was made 0.010 N acid with H§804 then made slightly alkaline, PH. 8.0 with NaOH. The settlement in this poor case was a186~§§§ as shown in sample 2 Fig 18. Fig. g, \\ Showing the effect of variations in the precipitation procedure on the slud e formmtion. (1) Haste made strongly acid and then brought back to PH 7.8. Note that part of the sludge rose to the surface leaving a cloudy effluent. 60. (2) Waste made strongly acid and then.braught to pH 8.0. Note the poor sedimentation. ’7‘0”, (3) Waste properly treated. Note that all §ES£25 settles directly to the bottom. (4) Untreated milk waste. The character of the effluent resulting from these variations from the regular proceedure can be Judged from the following partial analyses. (1) Total solids = 6100 p.p.m. Organic nitrogen 27 p.p.m. (2) (3) Total solids 1730 Inorganic " 580 Organic " 1150 Organic Nitrogen 36 (4) Total solids 2460 Inorganic " 260 Organic " 2200 Organic Nitrogen 159 Fig. I? V2“ --“ In: Same as Fig; QT after standing three days Note the increased thickness of the scum in No. l and 2 also the scum that is starting to form on No. 4 . Note, however that the appearance of No. 3 has not changed. The lowering of the level in some of the jars is due to the use of some of the effluent for analysis. . I { a n (1) Fresh 2% milk solution. (2) Milk solution after standing 12 hours. (3) 2% milk Waste after chemical treatment. 62 Effect of Chemical Precipitation on Bacterial Flora. It was eXpected that the precipitate in dragging down the suspended matter would also remove many of the bacteria that were in the waste. The following experiment proved this to be true. A 2% milk solution was prepared in a three liter jar and seeded with bacteria from various septic tanks, sewage, other milk wastes, etc. and allowed to stand two days, after which a bacterial count was made. The waste was then treated -;fi1§h§}afifial2w§3 by chemical precipitation and another analysis made. The decrease in bacteria is shown below. Dilution 1/100,000 l/loo Before after % remaining rotate 22,200,000 11,400 0.05% Acid 600,000 400 0.07 Alkaline 100,000 100 0.10 Neutral 21,500,000 10,900 0.05 Casein liquifiers 600,000 400 0.07 This decrease in the bacterial flora indicates that if the waste is to be further reduced after precipitation that it should be stored in a separate tank where bacteria will be free to develop, as otherwise the subsequent precipitations would continually reduce the bacterial flora. 63 Septic Tank Principle and Chemical precipitation While it is obvious from the preceeding experiment that precipitation should not be conducted in a tank used for subsequent storage of the effluent, a slightly different condition was tried in the following experiment. Three liters of a 2% milk solution were placed *6 in a four liter glass Jar shown in Fig.;_ F Once a day two liters were siphoned off leaving one liter in the jar. Two liters of fresh 2% milk solution were prepared in a separate vessel and treated with ferrous sulphate and sodium hydroxide, in the usual way. This mixture was added, carefully through the funnel to the one liter remaining in Jar (A). (H) 61+. ' When this process was first started, 100 cc. of the waste from the fixed pH. septic tank process was added after the precipitation in order to seed the supernatant liquid with bacteria. It will be seen,that in this experiment the precipitate had formed in the fresh 2% milk solution before it was added to the cue liter of waste remaining in Jar (A) (A) An analysis after several days of operation indicated that a good bacterial flora was being maintained. However A the highly acidified nature of the one remaining liter of old waste was sufficient to prevent good sedimentation}? a r A ¢ >£fi§§(The effluent was somewhat cloudy, scum formed on the surface and the effluent and scum had offensive odors. A typical analysis of the effluent is given below. Total Solids Grease Inorganic solids Organic solids Suspended matter Oxygen consumed. Organic nitrogen Bacteria/96¢ : Dilution l/lOO 1/1000 2580 p.p.m. O 475 2105 356 150 72.4 1/10,000 (rum 1 «M ow! Total --—Too thickr- 1,310,000 Acid ¥,/’/4 0 Alkaline 220x299 Neutral 1.100,000 Casein liquifiers 110,000 1/100,000 1,900,000 0 600,000 1,300,000 300,000 65 Results obtained when Chemical Precipitation is Properly Conducted. I I; §( When 2% milk solution is treated with 0.5 grams per liter of ferrous sulphate and brought to a Hydrogen ion concentration of pH. 7.8 a heavy gelatinous precipitate of ferrous hydroxide forms which settles out in about ten minutes leaving a perfeétly clear supernatantliquid.‘ (”X l suspended matter including all the butter fat and most of the protein and bacteria are carried down with the precipitate leaving a slightly alkaline liquid containing about 900 p.p.m. of lactose, about 200 p.p.m. of dissolved protein, and about 600 p p m. of inorga nic matter consisting of dissolved ferrousn hydroxide, excess calcium or sodium hydroxide and various salts. The effluent has a relative stability of about 60%,WfiifiHZLB/as”gggdwq§ the ‘3 ...... _A-“x ,. . '; \ /&Rflfiffiltertefifluentoat“Badleen«a A characteristic analysis of this effluent is shown. below. Total solids 1750 p.p.m. ll Inorganic Sol. 580 Organic Sol = 13:50 p.p.m. Grease - 0 p.p.m. SuSpended sol = 0‘ p.p.m. Oxy cons = ? p.p.m. Organic N g 36 p.p.m. Relative Stability =60% .——r-.—-.—- .-"-.- 66. p_ Upon standing two days considerable bacterial action 'Kj gages place. The hydrogen ion concentration rises to 5.8 and a reduction in the organic solids occurs. Total Solids = 1020 Inorganic " = 460 Organic " = 560 No odors develop during this period of storage nor at any later period. , It will be seen that this process produces directly a clear, fairly stable, nonoffensive effluent which in many cases would be considered entirely satisfactory. However if further reduction is desired the effluent is ideal for secondary treatment in a sand filter. Because of the easily oxidizable nature of lactose a high rate of application might be used. The Cornell University Experiment Station found that septic tank effluent could be treated at the rate of 100,000 gallons per acre per day. Theeeffluent from the chemical precipitation process being more satisfactory for sand filter treatment could probably exceed this amount. 5 One troublesome feature of the secondary treatment of creamery waste with sand filters which is universally astcxsfiwfi ff experienced is the constant clogging and the/frequent removal 1 of the scum infiggigflaegessggyvngiygfi -../W" V The absence of suspended matter in creamery waste treated by chemical precipitation would obviate this condition L. entirely, and a sand filter could su7€dsfully treat large 67 quantities of such effluent with practically no maintenance. Sludge . The dried sludge from one thousand gallons of creamery waste would contain about 2.7 pounds of ferrous hydroxide and varying amounts of butter fat, casein, suspended souids, and other organic matter. '1M€§3;?;ettles very quickly and may be removed soon after formation It soon dries, forming a dark brown, granular, odorless, inoffensive, substance. It is probable that it would have considerable fertilizing value. Conclusions from Chemical Precipitation EXperiments. {1) Milk wastes of high concentration may be very sucessfully treated with ferrous sulphate and lime. (2) For milk wastes of ordinary concentration the treatment should consist of adding 0.5 grams per liter or 4.2 pounds per thousand gallons, of ferrous sulphate, and then adding the basic materialuasadseacreihedLQQ messes ~ (3) The process removes the butter fat, suSpended solids, and most of the protein and bacteria, (4) The sludge will settle in a very short time after treatment and may then be withdrawn. 68. (5) The effluent will be clear and nonoffensive and “ '0/m’ld it may be discharged directly without fear of odors or offensive conditions arising. (6) The effluent from this process has a relative s stability of 60% but if further reduction is dedired it may be secured by storage in secondary tanks or by oxidization in a sand filter. RECOMENDATIONS FOR DESIGN OF DISPOSAL PLANT USING CHEMICAL PRECIPITATION AND SECONDARY TREATMENT. The Wastes from the average isolated creamery are small in quantity and highly concentrated. as is shown by the data onggegxaim. ~‘ ’ . J? This condition presents a very difficult problems: when ordinary disposal methods are used but is ideal for the economical use of chemical precipitation. From the data on /\ L\‘~fi42eg25 it will be noticed that many plants have less than one thousand gallons per day of waste. 4 1 For economy the waste egould be isolated from cooling andscondensery water and kept as concentrated as possible, consistent with convenience., /”,. _/’Fig'. 2; suggests a plant arrangement for an average creamery having five hundred to five thousand gallons of concentrated waste per day. .$e\\\\\m W Ee v.1 Oual.o Ills-anon: I 00.4 .- cup WIN-.uouvhl..vllv1‘l 4‘00”” .aoJfl-h eludP-luoone. . clan-1o c s. we... Ina-Ie ,- ... 4 \ ......tu... .................. ... . 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