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A study of the extraction of inulin from dried dahlia tubers

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A study of the extraction of inulin from dried dahlia tubers

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Content A STU D Y OT TH E EXTRACTION OF INULIN F R O M DRIED DAHLIA TUBERS A T hesis Px.eRent.ed to th e Sheulty of th e Department o f Chem istry U n iv e rsity o f Southern C a lifo rn ia In P a r t i a l F u lfillm e n t o f th e R equirem ents f o r the? Degree M aster o f A rts by W ilfre d M °Neill NoMe September 1937 UMI Number: EP41496 All rights reserved IN FO R M A TIO N TO ALL U SER S The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. UMI O f e s s r ta tf o f t: P u W is f in g UM I EP 41496 Published by ProQuest LLC (2014). Copyright in the Dissertation held by the Author. Microform Edition © ProQuest LLC. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code P r o te s t ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 4 8 1 0 6 -1 3 4 6 This thesis, written by IILE, B E D ...M .C .K E IIL L ..R Q B L E I........... under the direction of h-%3- Faculty Com m ittee, and approved by all its members, has been presented to and accepted by the Council on Graduate Study and Research in partial fulfill m ent of the requirements for the degree of M A STER OF ARTS Dean Secretary D ate............S e p t e m b e r . , - 1 9 3 - 7 -- Facuity Com m ittee nrma e y \ i ^ TABLE OF CONTENTS PAG E I INTRODUCTION ....................................... 1 H is to r ic a l background . 1 Tb© n a tu re o f in u lin , i t s so u rces and u se s . 1 P revious work done i n t h i s f i e l d . . . . 3 I I PROBLEM............................................................................... 6 Drying th e tu b e rs . . . . . .. .. 6 E x tra c tin g th e in u lin ................................................. 6 P u rity of th e product . . 6 I I I N O TE . * . . 6 IV EXPERIMENTAL WORK.......................... . . t. . 7 Drying th e tu b e rs .. . . .. .. . 7 D eterm ination of p ro p o rtio n o f w ater to dry m a te ria l f o r e x tra c tio n . . . . . 15 Study of re s id u e s , s o lu tio n s and use of calcium carb o n ate . 17 E ffe c t o f v ary in g th e tim e o f h e a tin g . . 19 E ffe c t of v arying methods of h e a tin g . . . 33 E ffe c t o f tem p eratu re on f i l t r a t i o n . . . 33 P u rify in g and f i l t e r i n g mediums . . . . 34 T RESULTS A N D CONCLUSIONS.............................................. 26 VI S U M M A R Y . . . . . . . . . . . . . 29 V II BIBLIOGRAPHY.................................................................. 50 LIST OF TABLES PA G E I Weight Lost in Drying Tubers . . . . . . 9 I I Per cen t of In u lin O btained Using D iffre n t Amounts o f Water in E x tra c tio n ........................... 15 I I I V a ria tio n of H eating P erio d in E x tra c tio n . . 21 IT Comparison o f Mediums . .................. 25 LIST OF G RA PH S I Drying curve A . ..................................... 10 I I Drying curve B ............................................. . 11 I I I Drying curve C ............................................ 12 IV Drying curve D ............................................ 13 LIST OF PLATES I D r i e r .......................................................... 8 I I Loss o f w eight p e r hour in drying . . . . 14 I I I A pparatus used in e x tra c tio n .......................... SO IV P ro p o rtio n o f w ater to dry tu b e rs . . . . 16 A STUDY OF T H E EXTRACTION OF INULIN FR O M DRIED DAHLIA TUBERS INTRODUCTION. I n u lin , Imam, a lso as a la n tin and d a h lia , was d isc o v e r ed by T a n ra t. S im ilar to s ta rc h , i t is commonly found a s a re se rv e fo o d s tu ff in s o lu tio n in th e c e lls a p o f some o f the Com positae. Most prom inent among th ese a re the tu b e rs o f th e d a h lia and a rtic h o k e and the ro o ts of th e c h ic o ry . A d d itio n al 2 so u rces are l i s t e d by Haas In h is book, "An In tro d u c tio n to th e C hem istry o f P la n t p ro d u c ts ." This Yfoite s ta rc h lik e substance i s of i n te r e s t as a source of le v u lo s e , into which i t may be co nverted by hydro- 3 l y s i s . C rookew itt was th e f i r s t to p rep are le v u lo se by t h i s method, h is work being re p o rte d in 1845, alth o u g h D ubrunfant sometimes re c e iv e s the c r e d i t . One o f the most prom ising so u rces of in u lin i s the d a h lia . The la r g e , e a s ily propaga te d tu b e rs of th is p la n t s to re a c o n sid e ra b le amount o f food in t h i s form., in some cases as much a s 16$ having been re p o r te d . 1 A rm strong, tf$he C arbohydrates" 209 1935 2 Haas, "An In tro d u c tio n to the C hem istry o f P la n t ,P ro d u cts" 1 ; 131 1921 3 C rookew itt, Annalen 45 : 184-192 1843 D ah lia tu b e rs are r e a l l y ro o ts and the term tu b e rs i s used h ere as a m atter of common custom . The in u lin i s h eld in s o lu tio n in the p la n t tis s u e beneath the pigm ent la y e r . The amount of in u lin v a r ie s g re a tly w ith th e n atu re o f the m o ts and th e time o f the y e a r, accum ulating d u rin g th e w ln- te r m onths. The la rg e «)uioy ro o ts g iv e h ig h er y ie ld s than do the o ld e r and more f ib r o u s . The usual method o f e x tra c tio n has been to c ru sh or g rin d the r o o ts , add a sm all amount of calcium c a rb o n a te , and e x tra c t 4 5 6 ? w ith b o ilin g w a te r. * * * * The s o lu tio n th u s o b tain ed may be tr e a te d by any one of a number o f d if f e r e n t m ethods.. The 4 5 in u lin may be p r e c ip ita te d by th e a d d itio n of a lc o h o l, * * 5 by fre e z in g , or by allo w in g i t to stand in a s u f f ic ie n tly c o n c e n tra te d form u n t i l p r e c ip ita tio n o c c u rs . The p r e c ip i t a t e i s th en re d isso lv e d and e ith e r p u r if ie d w ith anim al ch ar c o a l o r e ls e r e p r e c ip ita te d by means of a lc o h o l as many tim es a s may be n ecessary to procure a pure w hite p ro d u c t. The amount of in u lin reco v ered v a rie s from 3$ to 15$. The wide ra rg e i s due m ainly to th e f a c to r s which were m entioned above. 4 Thorpe, “D ic tio n a ry o f A pplied C hem istry” 1 : 655 5 Haas, opp. c i t . 134 6 Morrow, "B iochem ical methods” 7 M o lin a ri, "Organic C hem istry” , 2 : 533 The s tr u c tu r e o f in u lin i s s t i l l somewhat u n d e rta ln , alth o u g h most a u th o r itie s agree th a t i t is a p o ly sacch aro se c o n s is tin g o f about t h i r t y m olecules o f fru c to se ® Joined to g e th e r in g lu e o s ld lc lin k a g e ^ I t i s q u ite so lu b le above o o 80 C and extrem ely so lu b le above 90 C» I t farms sp h aero - c r y s ta ls . In u lin does n o t reduce F e h lin g ’s s o lu tio n , but may be d e te c te d by means o f G reen 's t e s t o r M o lisc h 's t e s t . I t does not r e a c t upon the a d d itio n o f an io d in e s o lu tio n , as does s ta r c h , but g iv e s a c h a r a c te r is tic brown c o lo ra tio n . T his must be compared v dth a s im ila r s o lu tio n co n tain in g no in u lin , fo r io d in e i t s e l f i s brown. There i s no com pletely s a tis f a c to r y method, a t p re s e n t, fo r the q u a n tita tiv e d eterm in atio n o f in u l in . Approximate r e s u l t s have been o b tain ed by c o n v e rtin g i t to le v u lo se and determ ining the le v u lo s e . The p o la risc o p e has a ls o been used the s p e c if ic r o ta tio n o f in u lin , according to Irv in e and S te e le , being between -35 °and - 3 6 °.10 A number o f w orkers11 have found from 3$ to 3 .7 $ g lu co se upon h y d ro ly zin g in u lin which su p p o rts the th e o ry th a t th e ch ain c o n s is ts o f from 86 to 30 8 A rm strong, opp. c i t . 9 Whitmore, “O rganic C hem istry” 586 10 R e ig e r, D octors T h esis, U n iv e rsity o f Southern C a lifo rn ia , Los A ngeles, C a lif o r n ia . 11 A rm strong, opp. c i t . fru c to s e u n its with, a te rm in a l g lu c o se . Osmotic p re ssu re mea- 1 2 surem ents show in u lin to have a ch a in o f 31 u n i t s . A ir d rie d in u lin is a s ta b le substance c o n ta in in g approxim ately 10 ft w a te r. In the e x tra c tio n of in u lin from d a h lia tu b e rs by the methods g iv en above, c o n s id e ra b le d i f f i c u l t y has been encoun te re d in f i l t r a t i o n . This has been shown to be due, in p a r t , to th e manne r o f p re p a rin g the tu b ers* R ieger3 * 3 has shown th a t speed o f f i l t r a t i o n could be in c re a se d by s lic in g the tu b e rs ra th e r than g rin d in g o r cru sh in g them. He a ls o ob- s e r v e d ^ th a t a t a tem perature of around 80°C th e re was a coag u la tio n o f p ro te in and albuminous m aterial, w hich did not ag a in go in to s o lu tio n , and t h a t other im p u ritie s were removed along w ith t h i s p r e c ip it a te . The work of D aily*^ on d eh y d ratio n of v e g e ta b le s , fu rn is h ed su g g estio n s as to methods which proved o f v a lu e . He noted th e f a c t t h a t th e re were p ro d u c ts w hich were more e a s ily se cured from the s lic e d d rie d m a te ria ls w hich were l a t e r powder ed . He a ls o noted th a t th e r a te o f d ry in g depended on the 12 G arter and R ecord, Chem istry and In d u s try ,218-19 1936 13 S e ig e r, opp. o i t . 19 14 Reigrer, opp. c i t . 45 15 D aily , L.R . D octor*s th e s le s , U n iv e rsity o f Southern C a lifo rn ia , Los A ngeles, C a lifo rn ia . n a tu re o f th e m a te ria l, th e tem p eratu re, th e r a te o f flow o f a i r , th e tim e, and th e amount o f m a te ria l p laced upon th e drying tr a y s . Another p o in t which he observed was th a t a drying tem perature of 55 ° o r le s s was n o t harm ful to the ma t e r i a l w hile one o f 70° o r over was in ju rio u s ; also th a t th e dry h e a t was le s s harm ful than the damp, Tubers d rie d in from 6 to 10 hours were in v ery good c o n d itio n a year l a t e r . These tu b e rs co n tain ed le s s than 5*3$ o f m oisture* 16 Huth has shown t h a t a y ie ld o f from 30$ to 37$ in u lin might be o b tain ed from th e d rie d tu b e rs . I f th e ease o f f i l t r a t i o n and p u r ity o f p ro d u ct ean compensate fo r th e c o st o f d ry in g , th is method of e x tr a c tio n becomes an in te r e s tin g in d u s t r ia l problem,. 16 Huth, S.H. Mas te r* s th e s is , U n iv e rsity o f Southern C a lifo rn ia , Los A ngeles, C a lif o r n ia . PROBLEM S in c e , in th e e x tra c tio n of in u lin , c o n sid e ra b le d i f f i c u l t y in f i l t r a t i o n had been encountered and sin ce i t was f e l t th a t th is was prob ab ly due to th e presence o f album inoids or o f fin e c o llo id a l, m a tte r and t h a t dry* ing m ight co a g u la te the album inoids and in c re a se the s t a t e o f a g g re g a tio n , i t was proposed in th i s work, to ; 1 . Dry the tu b e rs and e x tr a c t th e in u lin from them* 3* Study methods and r a t e s of e x tra c tio n * 3* L et erm ine, to some e x te n t, th e p u rity o f th e product* H C H C E In o rd e r to avoid the p o s s i b i l i t y of non uniform m a te ria l in th e se experim ents, a s u f f ic ie n t amount of th e tu b e rs was s lic e d , d rie d , and ground, to perform th e work, covered in t h i s re p o rt* EZPE RIM EH TA K W O R K Dry lag the Tubers The tu b e rs were sliced , to a th ic k n e ss of about !• § • to 2 m illim e te rs , These s lic e s were then placed, on tra y s in an a i r d ry er (see P la te 1} in la y e r s about th re e deep. They were then d rie d in a c u rre n t o f a i r a t a tem p eratu re o f ab o u t o 45 C fo r a to ta l o f 27 h o u rs. Four samples were tahen and th e ir w eights checked h o u rly fo r th e f i r s t e ig h t ho u rs. Two o f th e sam ples were th re a d e d on s tr in g s , and two were p laced on watch g la s s e s , (see ta b le 1) A fte r e ig h t h o u rs, th e ap pearance o f th e sam ples which were th read ed was th e same as th a t o f th e body of th e m a te ria l on th e tr a y s , w hile t h a t o f th e sam ples on the w atch g la s s e s d iffe re d m a te ria lly and was ob v io u sly not w holly d ry . Graphs showing th e r a te o f dry in g o f th ese sa u rie s,, (see graphs 1, 2, 3, and 4} and a c h a rt shew in g the h o u rly lo s s in w eight (see p la te Z \ in d ic a te c le a r ly th e r a t e o f d ry in g . The th rea d ed samples reached c o n stan t w eight in le s s th a n seven hours, w h ile the o th e rs a tta in e d i t during tbe n ig h t. T his a g re e s c lo s ly w ith th e r e s u l t s l 1 ? o b tain ed by D a lly . The s l i c e s were d is c o lo re d in t h i s d ry ing to some e x te n t, becoming s l i g h tl y browned. During the d ry - ir g , the tem p eratu re v a rie d from 43°to 52°due to th e la c k o f any means o f c o n tro l. 17 D aily , Ib id TOP 6000 Waits "H th Jr<»» 'I'ftH R 1"*** Drying Trays SIDE H eater D r i e r Plate 1 9 lEhreaded Samples A B Hows Weight o f lo s s o f Hours Weight of lo s s o f D ried Sample Weight D ried Sample Weight 0 3 2 .Ogms Ogms 0 32. Ogms Qgms 1 1 9 .0 13.0 1 22.0 10.0 2 14.5 4 .5 2 15.5 6 .5 3 9 .0 5 .5 3 10.0 5.5 4 6 .0 3 .0 4 5.5 4 .5 5 5 .0 1 .0 5 5.0 .5 6 4 .5 .5 6 4 .5 .5 7 4 .5 0 7 4 .5 0 8 4 .5 0 8 4 .5 0 2? 4 .5 0 27 4 .5 0 Samples on Watch G lass C B 0 35.0 0 0 37.0 0 1 26.5 8 .5 1 29.5 7 .5 2 21.5 5.0 2 22.5 7 .0 3 16.5 5.0 3 18.0 4 .5 4 12 .5 4 .0 4 14.5 3.5 5 1 1 .0 1 .5 5 12.5 2 .0 ( s lic e s turn ed h ere) 6 9 .0 -2.0 6 - 7 .0 5.5 7 7 .3 1.7 7 7 .0 0 8 6 .5 .8 8 6 .5 .5 27 5 .5 1 .0 27 5 .0 1 .5 E vaporated w ate r - 86$ D ried tu b e rs * 14$ • T ’ n'hTa 1 G ra p h ! 1 0 I B B B B B B B B B B B B B B B B S B i I B B B B B B ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ I B B B B B B B B B B B B B B B B B f l i ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ii£5i£5£££££££i£2iili!£ii££i££££££i£ I B B B B B B B B B B B B B B B B B B i B B B B B B f l B B B B B B B B B a I B B B B B B B B B B B S B B B B B B * B B B B B B B B B B S B B B B B B i S B E S E E E E S B S E E B E i E f l B S E B E S a S S S B B a E B E ! ISSESBEBBBSBBIBEBiiBIEEEESBIBSSBEEBES ia ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ * ■ ■ ■ f j k i i i f i a a i a a i i M i B i a i i B a a B B i i B B B B B a a a a i f i a a a a a a a a a a a a a a a a a a [ B B a a a a a a a a a a a a i i , / a i B i i M a a a B B B i B B B B i I B B B B B B B B B B B B B B i B i B B B I B B B B I I B B B I B B B I I [■ R l l i l V B B B B B B B B I I I 1 B I R M I I H B I I ■ » ■ ■ ■ ibbbbbbbbbbbbbbb? 1 Ab b b ib b b ie ib b b ib b b b i iSiiiE3iiiii£iiiiiii5£SIisiB££ssei SB! bebbbbesbsesee; L o I ' < s > s *0. 1X91. ; lt* l U t HIILIK. LOI IHXtLII cv N U > W eig h t in 6ram% Drying Curve Sample A T e*w p.= 42“ c Weight i n Grams T im e in Hours D rying Curve Sample B G ra p h 2 G r a p h 3 < 5 w < r > H O . 2101. JESEE R A Y H IL L E R . L O I A N S C L K f o CO Drying Curve Sample C Tem p. = 40*0 W eioh t i n G ra m s |M > m ) 2 T im e in Hours Drying Curve Sample D 9 it) hn — * 27 Temp - 43.5° C Graph 4 ith 9 • f o I f Sample A Threaded Sample B Threaded Sample C Watch Glass Sample D W atch G lass S I te e s I Ti/rned i.O t.5 1 0 Loss in Grams 1 0 to Loss o j W eight per Hour 1 0 15 The D eterm ination o f a S a tis f a c to r y P ro p o rtio n o f Tfater to "D ry M a te ria l f o r E x tractio n * Sinee an excess of w ater would d isso lv e p a r t o f th e p r e c ip ita te and to o sm all an amount would oause incom plete e x tra c tio n , i t was n ec essary to determ ine a s a tis f a c to r y p ro p o rtio n * The e n tir e amount o f tu b e rs were f in e ly ground, and a number of sam ples taken * To th e s e sam ples w ater was added in th e r a t i o s of 3 to 1 , 5 to 1 , 10 to 1 , and 15 to 1* These samples were th e n h eated on a w ater h ath a t an average tem p eratu re of 90° fo r one hour * The amount o f in u lin ob ta in e d from each is shown in P la te ''3* th e two sm a lle r amounts were e stim a te d , the n a tu re of the p r e c ip ita te making a c c u ra te w eighing im p o ssib le . The th r e e to one r a t i o y ie ld s n e a rly as much as the fiv e to one ; b u t the l a t t e r , b esid es having th e la r g e r y ie ld , i s much e a s ie r to handle and to s t i r because of th e la r g e r p ro p o rtlo h o f liq u id p r e s e n t. R atio W ater Tubers Per cen t In u lin 3 1 17 .5 $ 5 1 20.. 7$ .15 1 0 1 1 1$ to Zfo (e stim ated ) ♦5$ to 1$ (e stim ated ) Table 2 P late 4- 16 o c v v © 2 Per C ent Inulin O o 17 A Study of E re o jp ita tlo n W ithout the Use o f CaCQ* 250 gms of dry powdered tu b e rs were p laced in a 2 l i t e r beafcer w ith 1250 oc of b o ilin g w ate r, This was p laced on a w ater h ath fo r one hour and s t i r r e d c o n s ta n tly . I t was then f i l t e r e d , u s irg s e v e ra l f i l t e r papers c o n se c u tiv e ly , and washed w ith hot w a te r. In the follow ing o u tlin e , £ > In d ic a te s s o lu tio n and R, re s id u e . Solu tio n I {Residue 1) , (on n ex t page} Made .2 fo 12IC HC1 by v o l. allow ed to stand, overnight and f i l t e r e d . S 2 S 2 n e u tra liz e d w ith IKa^Gg Y/ashed w ith 5cc co ld made s lig h tly a c id to w a te r, d rie d and w eighed, litm u s w ith HG1 and W ei^it d ry , 28 gms. 1 .1 $ evaporated on w ater h a th . Residue hydro l i z e d , w t. ahout 100 gms. This re sid u e was d isso lv e d along w ith a number o f o th e rs , tr e a te d w ith R o rit and U l t r o l and f ilte r e d * S 5 R 5 D iscarded " ' " ' Titery Y/hite. 18 (s o lu tio n 1 on ___________ Residue I (preceding page} 350 ce w ater added and re h e a te d one hour? as above* F ilte r e d very slowly* S 3 ■ ___ R 3 Gaoled,, made »Zfo HCX by v o l. D ried and-we allow ed to s ta n d 40 h o u rs. Weight 93 gms:* S 4 . . R 4 E vaporated to Wt. dry 3gma dryness on w ater bath* s o lu tio n Weight o f th e h y d ro liz e d p ro d u c t, 71 gms The to ta l, lo s s of w eight was 157 gms* T o tal in u lin reco v ery S I gms. Wt of h y d ro liz e d p ro d u ct 190 gms* (in clu d in g w ater } Pec cent o f in u lin o b ta in e d 1* P er cen t h y d ro liz e d (e s tj This same proceedure was re p e a te d w ith the ex c ep tio n th a t 30 gas o f GaGQg were added a t th e tim e of heating* Weight o f in u lin in f i r s t p r e c i p ita te 71 gms P er ce n t in u lin * * ' " M 28*4$ The weight o f in u lin recovered in th e f i r s t p r e c ip i t a tio n .using CaCOs was over 23 tim es th e e n tir e amount reco v ered viien CaGOg was n o t used** I t w ill be shown l a t e r , t h a t th is is not due to th e p resen ce of calcium compounds in th e y ield * 19 The E ffe c t of Varying the Time o f H eating* To 1250 oo o f w ater heated on a w ater h ath were added 250 gms of tu b e rs and 40 gms of CaCQg* H eating was continued a t an average tem perature of 9Q O C and the m ixture s t i r r e d co n sta n tly * (see diagram of a p p a ra tu s, p la ^ e 3) A fte r the th ir d sample had been ta k e n , i t be came n ecessary to d isc o n tin u e the use o f the m echanical s t i r r e r and r e s o r t to hand s t i r r i n g due to the reduced volume* Samples were tak en a t 10, 20, 30, 45, 60 and 120 m inute in te r v a ls , f i l t e r e d 3 m inutes, and d iv id ed in to two p o rtio n s of 5 Q . cc each* One p o rtio n (a) was n o t chang ed* The o th e r p o rtio n (b) was made *2$ 12 m olar HC1 by v o l ume. These 12 samples were p laced in 50 oe g ra d u ates and allow ed to sta n d f o r 48 h o u rs. The volume o f th e p r e c ip i t a t e was observed a t th e end of 24 hours and d id n o t n o ti- e lb ly in c re a se during the second 24 h o u rs. A s lig h t ferm en ta tio n occu rred where no a c id was p re s e n t, none in the a c id so lu tio n s* The r e s u l t s o f t h i s experim ent appear in ta b le 3* A most in te r e s tin g o b se rv a tio n was th a t th e tu b e rs which were h eated fo r only 10 m inutes produced in u lin which was n e a rly as pure as th a t o b tain ed p re v io u sly o nly a f te r sev e r a l r e c r y s ta lliz a tio n s and th a t i t s w eight was l i t t l e be low th a t o f the samples o b tain ed by h e a tin g one and two h o u rs. Plate 3 30 - S T I R R E R - -TUBERS W A T E R BATH Time in minuses 10 2 0 3 0 4 5 “ 6 0 120 3 - na1 wrjl b -.2% H Ct a b a b a b a b a b a b Volume of the Preci pitcrfe-C-c. 3 7 3 3 4 9 4 9 4 % 5 5 0 4 9 4 9 4 9 4 9 5 0 5 0 v v t. of weT cake m grjms 10. s <f.5 /3 .5 “ 13.5 M-5* H »4 14 14 14 IQ > appearance of W et cake Creamy while iame 5am e Some Same Same 5«?m e S tf r r je Same Some Same 5 & e n e SpeeJ of Fi'ltrit io m I min | m i n L «>slhan 3 min 5 aero Sam e Some Same 5 jm c * Same Same Same Same W et'^h't «/ry 5 4.5* 5.2 5.2 6 6 5 .2 5 6 5.7 6 .5 6 4pp«aranee 7>ry white ft o ttly Starchy White Enf(V«/y Starchy L,$ht Brown granular Same Same Same Satrre Some Same Sacne Seme Same °J 0 ef S> ln (,) 1.0% .2% — — M o Trace — —■ — — M o M e Dvplitile i 0 *f*& (v 1.0% .2% — — A t Trace — — ■ — M o .2% Table 3 32 Methods o f H eating and Time o f F i l t r a t i o n of I n u lin . Three methods o f h e a tin g th e tu b e rs were t r i e d . F i r s t , to h eat fo r a s h o rt tim e; second, to s t a r t the s o lu tio n h eatin g a t a low tem p eratu re and to r a i s e the tem p eratu re; and th ir d , to heat the tu b e rs , allow them to sta n d fo r two h o u rs, re h e a t and f i l t e r them . In the f i r s t method, 100 gms of tu b e rs , 2Q gins o f CaCO g, and 500 oc o f hot w ater were p lace d on a w ater b a th . The m ixture was th e n h eated 15 m in u tes, f i l t e r e d and allow ed to stand o v e rn ig h t. On f i l t e r i n g the nex t day, th e tim e re q u ire d fo r the in u lin to re a c h th e crack ing p o in t was about 50 seconds. The y ie ld was not v ery h i^x and the product was lig h t brown and g ra n u la r. In the second method, the same amounts of m a te ria ls were used by the tu b e rs were placed in th e w ater a t about 7QPand th e tem perature ra is e d to 100P . The tim e h ea te d was ten m inutes. On f i l t e r i n g th i s s o lu tio n , th e same amount of p r e c ip ita te was o b tain ed as by the p re v io u s method but the appearance of th is p r e c ip ita te was s ta rc h i e r and w h ite r, when d rie d . I t was e a s ily brushed from the f i l t e r p a p e r. The wet p r e c ip ita te was c h a lk ie r and le s s s tic k y than most in u lin p r e c ip it a te s . Only 45 seconds were re q u ire d fo r f i l t r a t i o n . In the t h ir d m ethod, the same amounts were a g a in u se d . This tim e, the tu b e rs were placed in w ater a t a tem p eratu re 33 o f X O & fo r two or th r e e m inutes, h e a tin g d isc o n tin u e d , and th e m a te ria l allow ed to sta n d fo r a p e rio d o f two h o u rs. I t was then re h e a te d and f i l t e r e d . In th is c a se , the p r e c ip i t a t e was h e a v ie r than in the o th e r two. F i lt r a ti o n re q u ire d 60 seco n d s. I t was also f a i r l y easy to brush from the f i l t e r paper* I t was observed in the course of th e s e experim ents, th a t the in u lin which re q u ire d a lo n g er tim e f o r p r e c ip ita tio n was more d i f f i c u l t to f i l t e r and darker in c o lo r; th a t p r e c ip ita te formed in 24 hours f i l t e r e d q u ick ly and was l i g h t while, th a t d e p o site d from the same s o lu tio n on longer stan d in g was d i f f i c u lt to f i l t e r and dark, in c o lo r. I t was s t i c i y and, when d rie d , r a th e r horny. O ften th e p r e c ip it a t e which is o b tain ed on stan d in g over 24 hours i s so fin e th a t i t p asses through a #40 f i l t e r p a p e r. o ffature and F i l t r a t i o n when H eated a t 80 G 250 gms o f tu b e rs , 30 gms o f CaC03 and 125Q oc of w ater were h ea te d a t 8Q°C. Samples were taken a t 10 , 20 , 30 , 45, and 60 m in u tes. F i l t r a t i o n was q u ite d i f f i c u l t . The s o lu tio n s were allow ed to c o o l and made a c id a s b e fo re . The w eights in d ic a te d l i t t l e , , b ein g 10, 1 1 ,5 , 8*7, 10, and 12.5 gms r e s p e c tiv e ly . The c o lo r o f a l l p r e c ip ita te s was the same, being a l i g h t brown to stra w . I t was f e l t th a t f i l t r a t i o n d i f f i c u l t i e s were la r g e ly due to the d i f f i c u l t y o f m ain tain in g a h ig h enough tem perature d u rin g f i l t r a t i o n . P u rify in g ana F ilte r in g Mediums. A number of runs were made using: H o rit, a s p e c ia l form, o f c h a rc o a l, F i l t r o l , a c la y u se f o r p u rify in g :, and Speedex, diatom aceous e a rth fo r f i l t e r i n g , in d if f e r e n t com binations to determ ine which gave the b e s t r e s u l t s f o r p u r ity q u a n tity and speed o f f i l t r a t i o n . Since i t had been n o ted in p re v io u s runs th a t f i l t e r paper clogged a f t e r about 100 cc o f s o lu tio n had been f i l t e r e d , i t was decided to f i l t e r th e s o lu tio n through c lo th f i r s t and th en th ro u ^ i p a p e r. The r e s u l t s o f th is work appear in ta b le 4 , Each sample re p re s e n ts approxim ately 100 gms o f tu b e rs . In the l a s t sample in th e t a b l e , th e in u lin was allow ed to p r e c i p i t a t e , f i l t e r e d o f f , and re d is s o lv e d befo re being p u r if ie d . T his p u r if ie d p r e c ip ita te a p p a re n tly f i l t e r e d dry in a few m inutes, b u t, sin c e no crack s appeared, su c tio n was co n tin u ed . At th e end o f 25 m inutes no crack s had appeared, and f i l t r a tio n was d is c o n tin u e d . 35 Medium Time to F i lt e r Wet Appear ana e Weight Weight Dry Appearance 3fa F i l t r o l Speedex Ho a c id Emin* yellow 54 22 gray-brown. 3$ F i l t r o l 3$ Speedex »2fo Hoi 2 oreamy 54 22 lig h t brown 3$ H o rit 3$ Speedex Ho Acid 2 grayish, whit e 54 21 gray 3$ H o rit Z% Speedex .2 # HC1 2 g ra y is h w hite 54 20 gray 2$ H o rit Ho a c id 2 oreamy 72 25 g reen -y ello w 2$ H o rit *2fo HC1 2 w hite 67 25 green -y ello w 2$ H o rit 2fo F i l t r o l Ho ao id 1 w hite 50 19 f a i r l y pure 2f0 H o rit 2fo F i l t r o l ♦2$ HC1 1 w hite 49 17 f a i r l y pure 3fo H o rit 3$ F i l t r o l 3fo Speedex 3 w hite 79 29 lig h t yallow 2\$ H o rit 2fo F i l t r o l Added to cake 3 to 25 v ery w hite 70 25 Q uite p u re , w h ite . Table 4 2 6 RESUITS MD CONCLUSIONS Drying the Tub er s* Using th e ap p a ratu s d esc rib ed , (p la te 1} a tem per a tu r e o f 45?C and pXacing X m m to 2 m m s l i c e s not over th re e la y e rs deep, d rying to c o n s ta n t w eight i s accom plished in from 6 to 7 hours* The w eight i s reduced 86$ o r to about X/7 th e o r ig in a l weight* Threaded sampies g iv e more accu r a te r e s u i ts than those p la c e d on watch gXasses* The p ro p o rtio n of W ater to Dry M aterial* 5 p a r ts of w ater to X o f tu b e rs gave th e h ig h e s t y ie id aithough a r a t i o o f 3 to X was not bad* In te rm e d ia te r a t i o s might be even higher* Too sm all an amount of w ater raafces a g ita tio n d i f f i c u l t ; too ia rg e an amount, g iv e s a Xow yieX d, The Use o f CaGQg CaC03 u sed to n e u tr a liz e a c id ity , gave h ig h er yleXds and d id not g r e a tly in c re a se th e ash.; 12 sam pies averaging Xess th an *35$, X O Xess than ®*2$* The Time o f H ea tin g * The tim e re q u ire d to h ea t th e d rie d tu b e rs d u rin g ex tr a c tio n is much Xess th an fo r the fre s h ones* The w ieght o f in u lin produced by h ea tin g only te n m inutes was from 80$ to 90$ of th a t o b tain ed by h e a tin g fo r one to two h o u rs. In one run th e in u lin o b tain ed was undoubtedly p u re r f o r the s h o rte s t p e rio d examined ClQ m in.J A time of le s s th an 20 m inutes is recommended. 3 7 Methods and . Tem peratures. P lacin g the n a .te ria l in warm w ater and r a is in g th e tem p eratu re to 95° b efo re f i l t e r i n g produced very good r e s u l t s and is recommended fo r f u r th e r study* H eating th e m a te ria l fo r a sh o rt tim e, a l l owing i t to sta n d and c o o l f o r s e v e ra l h o u rs, re h e a tin g and f i l t e r i n g was also s a t is f a c to r y . H eating, fo r e x tr a c tio n , a t a lower tem p era tu re did n o t in c re a se the y ie ld and caused f i l t e r i n g d i f f i c u l t y . P u r if ic a tio n and F i l t r a t i o n , She p u re s t in u lin was o b tain ed by the u se o f 2$ H o rit and 2$ F i l t r o l used to g e th e r. In th e q u a n titie s employed, Speedex d id not n o tic ib ly a id f i l t r a t i o n , A h ig h er degree o f p u r if ic a tio n was o b ta in e d by f i r s t se p a ra tin g the in u lin from th e s o lu tio n , re d is s o lv in g i t in a a n a ll amount o f w a te r, and th e n p u rify in g i t , That p o rtio n o f th e p r e c ip ita te which s e p a ra te s f i r s t , is most e a s ily f i l t e r e d . This o b serv a tio n was in c id e n ta l and should be more s p e c if ic a lly examined. E ffe c t o f .2 # C oncentrated HC1, In a l l c a se s where th e a c id was n o t added, fe rm en tatio n was observed in about 24 to 30 h o u rs. The a d d itio n o f the a c id re ta rd e d th is v ery much though the amount of a c id was n ot la r g e . Another n o tic ib le f a c t was the g r e a tly dim in ish ed a sh c o n te n t when th e a c id was added. The decrease 3 8 in w eight of th e ash was over 75$.. This may have been due to calcium s a l t s b e irg d is s o lv e d . Sneed of F i l t r a t i o n . F i l t r a t i o n was by means o f s u c tio n in a l l c a s e s . #40 Whatman f i l t e r paper was u se d . The f i r s t f i l t r a t i o n to remove the tu b e r re sid u e s was sometimes through c lo th , but th e s e s o lu tio n s were im m ediately r e f i l t e r e d th ro u g h p a p e r, Speed of f i l t r a t i o n was found to be dependant upon th e tem p e r a tu r e , the volume, th e r a te a t which th e in u lin p r e c i p i t a t e had formed, and whether or n o t th e p r e c ip ita tio n was com plete a t th e tim e of f i l t r a t i o n . In removing the tu b e r re sid u e s, f a i r l y ra p id r e s u l t s were o b tain ed in l o t s around 3Q Q gms o f tu b e rs by u sin g f i r s t th e c lo th and then th e p ap e r, th e whole being accom p lis h e d in around 20 m in u tes. In ca ses where th e s o lu tio n o b tain ed was 100 ©c o s c l e s s , f i l t r a t i o n was alm ost Im mediate; re q u irin g n o t over 5 m inutes. When th e volume was over 100 ©c th e paper dog g ed .. In u lin p r e c ip ita te s which formed ra p id ly and com pletely f i l t e r e d slo w ly . Those v h ich were f i l t e r e d b e fo re p r e c ip ita tio n was com plete f i l t e r e d q u ic k ly . P r e c ip ita te s up to 20 gms dry w eight f i l t e r e d in 1 to 3 m inutes. Speed was n o t n o ti- c ib ly a f fe c te d by the presence of th e HCI. 39 3 T IM M A E Y The r e s a l t s of t h i s in v e s tig a tio n o f th e e x tra c tio n of in u lin from d rie d ta h e rs in d ic a te t h a t : 1 The p a r ity of th e f i r s t in u lin p r e c ip ita te ob ta in e d i s b e tte r th a n t h a t from the f r e s h tu b e rs . 3 The tim e of h e a tirg “ fo r e x tra c tio n is about one fo u rth the amount u s u a lly r e q u ir e d . 3 A s a tis f a c to r y p ro p o rtio n o f w ater to tu b e rs fo r e x tra c tio n s i s 5 to X. 4 GaCQg in c re a s e s yieXds w ith l i t t l e in c re a se in im p u ritie s . 5 In sm a ll q u a n titie s * f i l t r a t i o n is more ra p id than when th e u s u a l method o f e x tr a c tio n i s employed. 6 The use o f m Zfa C oncentrated HCI re ta rd e d ferm enta tio n and reduced the amount o f a sh . BIBLIOGRAPHY BIBLIOGRAPHY Armstrong, E .F . and K .F ., The C arbohydrates. 1934 Haas, P au l, The Chem istry of P la n t P ro d u c ts, 1931 G a rte r and Record, Chem istry and In d u s try , 1936 C rookew itt, A nnalen, 1843 D aily , L. R ., D octors th e s is , U n iv e rsity of Southern C a lifo rn ia , Los A ngeles, C a lifo rn ia . H uth, S .H ., M asters th e s is , U n iv e rsity o f Southern C a lifo rn ia , Los A ngeles, C a lifo rn ia . M o lin ari, Organic C hem istry, Morrow, Biochem ical L aboratory Methods (?) Thorpe, D ictio n ary of A pplied Chem istry. Whitmore, Organic C hem istry. R ieger, D octors T h esis, U n iv e rsity of Southern C a lifo rn ia , Los A ngeles, C a lifo rn ia .

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Creator Noble, W. M (author)

Core Title A study of the extraction of inulin from dried dahlia tubers

Degree Master of Arts

Degree Program Chemistry

Publisher University of Southern California (original), University of Southern California. Libraries (digital)

Tag chemistry, organic,OAI-PMH Harvest

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Advisor [illegible] (committee chair), Johnstone, George R. (committee member), Stabler, Laird J. (committee member)

Permanent Link (DOI) https://doi.org/10.25549/usctheses-c17-789232

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