ADSDRPTIDI BY (SHARED! var-.1313 m EVELYD 5%: “CM coon muons 'x .4 ‘. . ' D {-11 -s" L: Y I n j ‘ ‘I'l’ "W: . (1". ‘l ’ '4'." ‘ "4‘ \ ~ . a . Lg. . . ‘ I ' O "i A L41. .1; 9. .‘r' ;’.‘7 . “- I.'|' . A. . ‘ T5! “ \'-‘ ”1. ‘ _‘ 1.. ‘I~"“}d"‘ - "‘l‘.‘ .. ‘." . '. . ‘l 0"", 3.. ' ‘ ; I ,-‘ .1) . L“) I ' ‘VL‘ ‘. . . _.‘ ‘~. \rvg. .“ 12 r:‘ 'I ‘i I ‘. . 3 ‘ \5. 5‘3“,” ‘c .9. $ ‘P b? '4‘: .‘ ‘ 1 .A‘ _ . 2 '9 _ ‘ p ?\ o 4 ‘ 4' M31? '- x 015}. “ V p .3 v .< < a,” . , J , . ‘ ._‘F‘ “$3. . ‘ .4 .1 , Hail—I" J . ’.“ ¢. . gs! . ,'.‘ ;-. . .. ‘, I?‘ICOF - :‘l'LTV \ ~ I f \ ‘1. V V . .a 1.gw4¢ym,_n I - . .v_ v}: - .- ,r “‘8‘" . 1.0" ?l‘ k0 ’1'.3 . ‘ ."c .l . . ' r, \ ‘.(. . 1 ' .. 2% ML" 7‘ *. *u 7.- k. 1 ' 3.- r— e: u . \ 4| *- V‘ ‘r.'-P.|:V‘ ¥ . ' "pg, 13-31” L §, A ‘ If. 5 " ,r ~2.‘ .L . "F {W}, fix... sick . . ~ - f t. (.3 1 '. | {.2 ‘ 7. \T‘J’r- a» . ‘ .11; J... 1‘5"“ '}f&-."- 1 . '1- .. , 1" L l".‘ ‘ " a" w . a .-' new: arr-h ‘ “rain ’31.“- ~‘E‘z‘n’”~ ‘I ___‘ . ;‘-‘ ‘rii‘. V t .j. , 3r.) ’ "y " . ‘ A -,.7Y.~"0 » o. . .- 2." f .. "(a‘fim-Gfir" ,‘ra‘z . - 1 -) ax. "fl- -‘d .1" at ”V. t f. hat-no .- ., _:.,. .5 .2 4",. 3a: {‘5}. ‘ "$- 2}? " 0 .j {#3. ‘ l . ‘ . .L ‘ '.""‘;&4’-.’" . . ‘ ‘ V . ,§ - n .+ 1. ’fi . ‘ "flit Ln 3' . VF ‘ ‘ ‘ . ‘l -‘ ' 'I . 'f": “'1" am 1'1 hr ADSORPTION OF LACTIC ACID BY CHARCOAL AND SILICA GEL A Thesis Submitted to the Faculty of Kichigan State College In Partial Fulfillment of the Requirements for The Degree of Master of Science BY r Evelyn.Cornman /'; Department of Chemistry 1933. T’T. L: A CHV'M IL. T {1‘1” 1,, : . T a" a l C 131:1 \ aw- ‘4-‘1 C; . ML I wish to eXpress my sincere atpreciation and gratitude to Dr. D. T. Ewing under Whose supervision this thesis was made possible. Evelyn Cornman ABSORPTION OF LACTIC ACID BY CHARCOAL AID SILICA GEL The phenomenon of adsorption was first observed about 1777, by the Swedish chemist, Scheele, tho noted that charcoal exhibited the property of retaining arious gases Without undergoing any apparent chemical change. Later,Lowitz (C.F.Ostwald, Lehrouch alleg“. Chemie, 2nd Ed. I, 1095 (ld9l)) made an even more startling observa- tion - i.e. that charco l t:;kes up dissolved substances from solution and retains them as it does gases. These two investigators opened up an entirely new field of research and since that time a vast amount of pork has oeo n done along the line of adsorption, great aivances having been made during the past 20 or 25 y ars. hot only has charcoal been used as the adsorbent, but kaolin, clay, fuller's earth, silica gel, finely divided platinum, etc., as well. Freunlich, Gibbs, Langmuir and others have advanced new t1 eories of adsorption, but thus far no satisfactory ex- planation of the nature of the phenomenon has been wholly accepted. Langmuir's theory of adsorption ( J.Am.Chem.Soc., 58 2267 (1916) E9 1885 (1917))a sumes that the forces act- ...” —.— ing in adsorption are nearly the sane kind as all the iorces causing chemical combinations. The atomic forces seem to be develOped from deviation of the orbits of the outer electrons in the atoms. The forces acting in ordinary chemical reactions are the result of the large deviations of these orbits, whereas in adsorption the forces acting zould be due to congaratively'small deviations. Langmuir further assumes that on the surface of a crystal there are a certain number of points where there are residual valen- cies and that adsorption consists of a fixing of the adsorbed atoms at these points on the surface, each point or space being able to hold one atom or molecule so that the adsorbed layer is only one molecule in thickness. Another adsorption theory of quite the opposite view is that advanced by Bucken (Ber., ;§, 545 (1914)) and Polanyi (Ber., lg, 1012 (1914), ;§, 55 (1916), Z. Elecktrochem.,§§, 370 (1920). This theory assumes that the outer layer con— sists, not of a single layer of atoms or molecules, but of a polymolecular layer with the density varying continually from the adsorbing surface out into the free gas or liquid. These are only two of the many theories that have been advanced and thus far experimental evidence is not sufficient to warrant acception of any one theory. However, it seems plausible to assume that in adsorption, surface forces pre- dominate. It is possible that chemical reactions may occur, but with fairly dilute solutions there seems to he no reason for considering the process to be other than that of surface condensation, which is adsorption. It has been found in the case of adsorption from solution that if the amount adsorbed from the solution is plotted against the concentration of the solution a curve concave to the concentration axis results. The slope of the curve varies with the adsorbent material as well as with the solutes and solvents used. A large amount of eXperimental work has been done in determining isotherms for such organic acids as oxalic, acetic, tartaric, but comparatively little has been done with lactic acid and in so far as lactic acid is supposedly oxidized by bone black (Boll Soc. ital. Boil. sper., §_, 884-7 (1927)) and decomposed by ultraviolet light (Z. physi— cal chem. ZIJ 311-4) it was thought desirable to reinvesti- gate its behavior and to determine whether or not it acted like other organic acids. method of Procedure and Experimental Results One gram of activated silica gel was allowed to stand in contact with 100 c.c. of Lactic acid solution for at least 24 hours, but if any adsorption occurred it was so slight that it could not be determined by ordinary titra- tion methods. A similar sample of activated silica gel was then evacuated and allowed to come in contact with another 100 c.c. portion of approximately .5 N lactic acid. Again there was no evidence of any adsorption. Failure to obtain any appreciable amount of adsorp- tion with silica gel necessitated substituting charcoal for the adsorbent. Norite, sugar charcoal and an activated commercial charcoal were tried. The lactic acid was 85% aqueous solution and had a Specific gravity of 1.21. A definite quantity of solution, of known normality, 100 c.c. vas placed in a glass stopper- ed 125 c.c. Erlenmeyer flask containing an accurately weigh— ed amount of Norite, 1.000 gm., in each. The flasks were shaken vigorously for approximately 60 seconds and then allow- ed to settle, in a constant temperature water bath at 250 C a: .0020 C.for 24 hours. The concentration of the solution was then deterndned by titration with sodium hydroxide solu- tion,using phenolphthalein as an indicator. The amounts adsorped represented by §_(grams of solute adsorped per gram of charcoal per 100 c.c.msolution) in the Tables are not Strictly accurate inasmuch as no attempt was made to correct for adsorption of solvent nor for the volume change due to adsorption of the solute. The unavoidable presence of CO9 would also introduce further slight inaccur- acy. Trial 1. Trial 2. Before Adsorption .000373 .001447 .006854 .0137 .0275 .0691 .1383 .2740 .5212 .0002308 .0004315 .001920 .003845 .0189 .0373 .0738 .1869 .3715 .5585 .7408 TABLE I . N. After Adsorption .0008554 .0005675 .0007962 .004272 .01220 .0521 .1204 .2590 .5019 .001054 (Basic) .0008797 " .0002834 .0003173 .0049 .02088 .05135 .16848 .3584 .5469 .7397 Bflfi .01107 .01814 .055 .0855 .1382 .1503 .1606 .1351 .1735 .01157 .01181 .01985 .03177 .12628 .14867 .20268 .1663 .1184 .1039 .1038 The results in Table I are plotted in Figure 1, Trial 1 represented in black, Trial 2 in red. The curves represent the average slope of the adsorption isotherm of Norite and lactic acid aqueous solution. Trial 1. Trial 2. N. Before Adsorption .0123 .0225 .0380 .0484 .0923 .1246 .1467 .1511 .1881 .00927 .0188 .0401 .0588 .0702 TABLE II. N.After Adsorption .0023 .0088 .0196 .0317 .0738 .1036 .1240 .1298 .1638 .00100 .00561 .0198 .0362 .0536 The results found in Table II are 2, Trial 1 is in black, Trial 2 in red. X .0900 .1226 .1662 .1506 .1662 .1891 .2041 .1922 .2182 .0744 .1189 .1827 .2027 .1494 plotted in Figure MICHIGAN STATE COLLEGE DEPARTM ENT OF MATH EMATICS MICHIGAN STATE COLLEGE DEPARTM ENT OF MATHEMAT le TABLE III. Trial 1. N. Before N. After X Adsorption Adsorption ‘E .00554 .000950 .0413 .02534 .01267 .1141 .05504 .03920 .1426 .1049 .08712 .1604 .2059 .1845 .1925 .3009 .2811 .1783 .3960 .3722 .2148 .4989 .4752 .2148 .6019 .5758 .2345 Trial 2. .00554 .000712 .0435 .02534 .01267 .1141 .05504 .0376 .1569 .1049 .0863 .1676 .2059 .1845 .1865 .3009 .2811 .1783 .3960 .3722 .2148 .4989 .4752 .2148 .6019 .5821 .1783 The data in Table III, plotted in Figure 5, gives a more characteristic curve than is observed in Figures 1 and -7- MICHIGAN STATE COLLEGE DEPARTM ENT OF MATH EMATICS 2, but there are still discrepancies that cannot be account- ed for by eXperimental errors. TABLE IV. NkBefore N. After §L_ Adsorption Adsorption m .009725 .001814 .0714 .02268 .00907 .1225 .04025 .0258 .1480 .06465 .0464 .1655 .08751 .0680 .1755 .1082 .0875 .1889 .2120 .1905 .1940 .5084 .2880 .1858 .4159 .5954 .1858 .8164 .7994 .1551 Figure 4 (results from Table IV) except for the points at .108 N, .212 N and .508 N gives a characteristic slope for Norite and lactic acid, but the curves given in Figures 1-4 are at such variency with each other that it was thought desirable to attempt a further activation of Norite. A quantity of charcoal was placed in silica dishes, covered and heated in an electric muffle furnace for three hours at a temperature of 5000 C. After heating it was NMCFHGAN STATE COLLEGE V—v—Var—qr ' VY V V Yfir fv v V V 'V ' V V I Pvt .. 1.1.111 .1 131*" 7- ”7T. T~TTTfo-T‘TI#«3--fi 1‘, , -LA l‘gyo—v. <9?» ...; . 2.0.. TI. . .«t4 It.+-...-I2 -....4.... . .. +47 4 69.¢oo .7... .5. 00. .v. 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I... ... . . .4 bra-*m—o . .1 . oi — ... . -.. . .4 ,.. ,a ...1....... .—. oocv . . , ‘y >r¢.§.>o., . ‘ ~uokr0.v A; f o-0~.or.:o -.4 .1 §2+4 . '4 I 4..-,o1.r... - .4 14' ..11..,, t, 4. A .1 -On ~-.>o—4 we '0'. 9'...A.a. 1,.¢o—.¢0. ~‘I'T'I' ‘I' ~r...._4 ‘ ‘ .3 9’.» IQ'fi004 .Il".lr'..+. OAf‘OfifOV " -‘ '94 Y I ‘ ‘ .9 .¢.,..yq...... ..Ay .».‘ ..6 . 1. .4~- .- .- y..+.—I—o—i—$——~ «fi-T p .— 9.. f 1— Hfi~d4~++ 9 >~~¢¢ ta 5161 Q . 4 < . . . , , - . o . . . _ . 1 . . - . . .- - o 1 1111 1 L-- A 1.1 4 1 .1 .1 A L LL “AICACAAS +........-...~.I.d_.¢_-a.4 DEPARI MENT OF MATHEMA‘I ICb allowed to come to room temperature in a dessicator. The following results were obtained when the acti- vated Norite was used. TABLE V. Trial 1. N. Before N. After 3g Adsorption Adsorption m .10692 .08534 .1943 .22438 .19863 .2208 .4487 .4217 .2430 .6621 .6376 .2208 .8975 .8632 .1545 Trial 2. .000888 .000 .0080 .00413 .000186 .0355 .00850 .00148 .0632 .0207 .00643 .1273 .0423 .02225 .1808 .0823 .0608 .1942 .2059 .1802 .2318 .5493 .5227 .2391 .8141 .7945 .1776 The curves in Figure 5, black line, Trial 1, red line Trial 2, from Table V come nearer to coinciding and are more regular than those obtained in any of the previous -9- MICHIGAN STATE COLLEGE _‘ -1. DEPARTM ENT OF MATH EMATICt Trials where the unactivated Norite was used. It will also be noted that with the activated Norite the amount of adsorption is greater than in the cases of the unacti- vated material and so it can be concluded that activation increased the amount of adsorption as Well as producing more uniform results. TABLE VI. N. Before N. After I: Adsorption Adsorption m .0044321 .0000713 .03926 .00908 .00108 .08103 .0823 .0621 .1820 .2086 .1848 .2141 .4151 .3902 .2234 .6291 .6031 .2236 .8366 .8107 .2236 The data in Table VI was obtained from a final Trial using the activated Norite and the plotting of these re- sults -Figure 6 - gives a curve that coincides with all the eXperimental points and resembles the isotherms character- istic of other organic acids. Several Trials were made using sugar charcoal that had been treated in the same way as the Norite. The follow- ‘lfl- MICHIGAN STATE COLLEGE o‘ DEPARTM ENT OF MATH EMATICS ing results were obtained. Trial 1. Trial 2. N. Before Adsorption .00443 .00908 .04486 .0823? .2086 .4151 .6291 .8366 .00526 .01053 .05215 .10483 .2602 .5204 1.0388 TABLE VII. N. After Adsorption .00302 .00681 .04080 .07945 .2043 .4118 .6269 .8366 .00368 .00842 .04872 .10009 .2539 .5141 1.0335 X. 111 .01265 .0244 .03649 .01629 .0389 .0292 .0194 .000 .01423 .01897 .03834 .04269 .0569 .0569 .0474 Figure 7 depicts graphically the results found in Table VII, Trial 1 is in black, Trial 2 in red. It is prob- able that the curve obtained from Trial 2 is the more char- acteristic. -11- STATE COLLEGE MICHIGAN ‘1II1'I l t. ‘1 lall.l|l ‘illjl. «I‘ll! . o . v . A W. 7- . . . . . v o v. . a . . . r9 ql. . ‘11. >—A -p— b—h—Q— 9—. . .. o .. V k .0 o i . v... j'l' T.. V r.. Y.“ Y.§V ’ ‘4 g ». ’_. . T o o o . . A 1 V 4 O 10‘. ... ¢oo1 A» . i ......o bu-voO—q-oooa 4 l . v . .1 n _ $. *o. ..... O I. b..- _ lo}: .4 . . 1.10! 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WM.¢~_..-. ~ -4 ,. ..y.. .. ‘ . . . . n . > 4 . . . . . 10 1:6-.. . _ . . . . . . . . . . . ..r. .Yivloll [- o... .,.+. ...v.. .. r.1._ ..... ... . . . . . . . . . . . o . o s . . . . . . . .. . ... A. u. . . .. .v .. ... .. p. ,l l, .. . .. ......, . ~ .. a. ... . ... .....A .. r.. A rllfi. . l ‘6‘ C o 1 . -‘IV- \~~-—. J1'.! II type! V 9 1.1, am; >-. -1 ...o a“; .72“ l a... ... .9..H .... ....* ‘06. ....w v.3. 6.00” >> . . b . Maui“; .- i . t . . v c .. . . , V...—.—¢.. 4.. . ._ .4. ._.v .i.‘ .0.” v .1. i. . _ . . -ovoo -o-+..o . . . . . o . a . | . It It . o o a 1 t o c . a. o .ql . .4 .v r. so #4 .9... 99.1 a... 4&6- 4...?A .444 oosol o.¢o .0.4L +vooA .o... .o. .1 o.. 0. ..~ p; v 0 v¢>-. a. DEPARTMENT OF MATHEMA‘I ILL: .h.»__ ._~ L-A.A o .. a 00“ ...o 5.09 con. 40.. 339. row» .ooo 401.. >053 v~¢& o... O6<4 .a... Q~4o ¢.++ .4.“ Man» Finally, a third sample of "activated" commercial charcoal, in pieces of approximately 1/8 inch in diameter was used. This was first ground and screened through a 100 mesh screen and then activated as in the case of the pre- viously used charcoals. The following data was obtained. TABLE VIII. N.Before N. After 3g Adsorption Adsorption m .00526 .00273 .02277 .01053 .00674 .03415 .0521 .0437 .0759 .1048 .0927 .1091 .2602 .2454 .1328 .5204 .5057 .1328 .7765 .7628 .1233 1.0335 1.0219 .1043 The curve obtained from the above results - Figure 8- is of the same nature as those obtained with sugar char- coal and Norite. Figure 9 contains 3 curves, the one nearest the con- centration axis represents the isotherm for sugar charcoal. (Table VII Trial 2) The curve furthest removed from.the con- -12.. 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' . q. . . .... ~' >‘> ‘ . . . --l. .. .. .|\.. ... .. ....~. . 1 . .... . . .. ' . - .. .. 4 .... _‘> . l _ "b .| H—pfivk _,._._J. , n~ —.-v-' .1 .. 9.4 e v .- ' - v. .5. .. . .l.- -. . ... .. . . .1 .. . . ....4 .1 a o n . ‘..... 1‘ ~«... ». ~ 0‘ .......' .A.,....¥. on . .Y.» ,-... .-. ..-o f .. -o4 5‘05 ..'n»..}.. -.c..f . n -I yvo - A . . .. “..U ’ -O 1 .A- 4 Av . . J‘AL4L“‘ AL—p-'=_—.—- L... . LJ.__.j.‘. ._. ..kJ-- ".-;-L~J DEPARTMENT OF MATH EMA Tle MICHIGAN STATE COLLEGE DEPARTM ENT OF MATH EM ATICS centration axis is that of Norite (Table VI). The curve midway between is that of the commercial charcoal (Table VIII). Discussion of Results The fact that silica gel failed to show any adsorp- tion or lactic acid was unexpected, but when we consider that silica adsorbs bases preferentially and inorganic acids not appreciably, the results obtained are more easily ex- plained. F. E. Bartell and Ying Fu (J.Phys.Chemfl§§, 676-87 (1929)) state that silica gel, free from impurities, is cap- able of adsorbing not only lactic acid, but other organic acids as formic, acetic, prOpionic, butyric, succinic, tar- taric, benzoic, and salicylic acids from aqueous solutions. However, the amounts adsorbed in most cases were so small with the exception of benzoic and salicylic acids that the ’5 amounts could not be determined by the method or titration used in this case. The adsorption of benzoic and salicylic acid was approximately 15 times greater than in the cases of the other organic acids. This they state is due to the fact that these two acids are but slightly soluble in water. If an organic solvent is substituted for water the amount of adsorption is greatly increased. -13- From the results obtained Nith harcoal as well as with silica gel it is evident that lactic acid in a ueous solution behaves as many othgr organic acids under siz' ilar conditions. When the activated charcoal was used t' ical ‘J 4 'C) isotherms were obtained. In a nuzfcer 01' the isotherms it is noted that as the solutions became more concentrated, from .5 H to l N there is a sli511t tendency for the amount of adsorption to decrease. It is possible the t this is due to a chemical deco position of the lactic acid by the charcoals. Further investigation on this phase of the subject mi5h prove profitable. It will be noted in Ei5ure 9, there a typical isotherm for each of the charcoals used are compared, that Iorite is capable of retaining a larger amount of acid th.n either 0: the other two. Some of t‘is is only an apparent adsorption ,__\ for it was found that the Norite used was of a basic charac- ter. lOO c.c. of distilled meter that has been in contact With 1.00 gram of Iorite for Zé hours reiuires 1.08 c.c. of .l N Eyf roclloric acid to neutralize it. Therefore some of the acid disappe““ing from solution must have been used to neutralize this basicity. Another reason for the greater adsorptive power of Iorite may be attributed to the size of the particles of carbon, the iorite used being much more finely divided than either the su.r 5ar charcoal or the commercial charcoal and hence having a 5reater available surface area. -14- bl} M0 wzsmo - .N101977 JUN 1 1 1997 n a m n I O c . v . I , k . p . I. \ . ' u.. . \ . \ . . . u. . . . . . . .l - . . \ . . I .. III . v 1 Q . O . . . .5. . . 1.. y I .l" x / a 4 . u . . r . \ ... . . 1..) 1' A D » . .... . .. .0. 1 I 1 \ . ~.-I . u ' l c L . . J .. . \. . . I I . . . O.. . , p . v . .. . ._ . - u v . .. .n I . . . . . . ... .. . .s L . . ... 0... I. . a. .. . 1 . .. .. . . .. .. r. . .. _ ...I- . . . u ,‘ . 1- f . . . x s, f- , . . .. ..... v; . ., . .‘v-v . I ~ .. 5 . _ u 1. . x. .r. . . Q .I .1 i I . . l O . v n .- . . .. a .- .1 \. . . «1 .. I u 1 I . I . . r/y . . . . . . o .\.. I . . . . x f V . . . . u .I. .. , . I u‘ u, H . . . k inks» ..L< 7 '. .o . u r. . . I . . 1. .v. 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