RAI'PISOSII(IIVDRATI:): Trisncclinride, C ~ x l i ~ O l a 51I& 20 Spccific rototion I Q ~ D
+ ............ ......................
..
Ash. ,
+IO.+.GO
hloisturc. . . . . . . . . . . . . . .
Ix I IA 51NOSIC ( 1I Y D WAT13)
(26.00 R per 100 & . )
0.10 pcrceht 0.15pcrccnt
:
3Icthyl p c i i t o s e , CnlIi101 specific rototion Itxl'$I Ash.. .\loislure,, , , , . , . ,
1110
.............
............................. . .. , , , . , . , , . , . , ,
- t 8 . 3 i o (0.~1.1s 8. per IOO cc.)
0 . 0 5 pcr cent (J, 10 pcr c e n t
,
SOK H Ir 01,: I Icxah ydric u lcoliol, CaTI;dh AI, p. (1 molccule HIO) , (0.5I n o ~ ~ c n uo ~ c) (nnliytlr OLIs) A SI1 I Aloisture.
'
.. .
750
................. ... ........................... .........................
1100 0 . 0 5 per cent 0 . I5 per cent
V:ec ironr rcducitig sugars SucRUsri:
l>isnccharitic, CizOti011 -0 Spccific rotiitioii la];, ,, Ash.. Moisture.. F r e e Irom rcduriiig sugurs
.
.................. ........................
.
+OO..i"
( 4 . 9 5 ~per . 100cc)
0.05 pcrcciit 0.0Gpcrccrit
sY I.(.JSfC ,<lopciito.;c, C~IlieOa (c:rllccl d.xyloRc.) 20 Spcciric rotntioii [ a ]0
.............f l B . 5 '
.. , ., ., . , .. ...... hfoistiirc ......................... --
,\SIl.,
____AI__-.-
by Fiscltcr 1-xylow, iiiorc proricrly
,
The Standardinition of' ltczre Sugars'
( 1 0 . 2 3 9 . ~per . 101) r e . ) 0.0; pcr wilt . . . 0 . 1 0 pcr c e n t .
is cli:trrctl and CC.ZSCS t o froth, arid thcn plnced in n muffle furii:ice, tlic muffk of wliicli is quartz. The heat is evenly distr:!xt.ed ovcr t>Iicbottoni of the rnume by incnns of Fisher
I.)urncrs.
,I tl:zrmocouplc, protected by a vit'reosil shell,
r e s k on the bottom of t,lic rnuffie, a n d connects witli a Brown recording pyroincter. The temperntiire of thc muffle is licld :it, cJ,ull red heat, or bctncen 1100' to 1200" P., for 2 hrs. I Iic :iiiiount of s u p r t:iken for tlic dctcrniitiation oE ash is I n
:dw:iys uniform, :inti by incans of tiic above cquipmcnt the tci1ipcr:iturc :iiici time of nshing are accurately controllcd. r . I lie :ittcriipt is itiadc to havc our sugars ns new ashless as i t is possii)lc t,o iii:ike tlicm. ~rois.i.r;rii+-'~lie inoieture detcrininntions of these rare sugnrs :ire iiot cntirely satisfactory, on account of four factors: hygroscopicity of some or tlic siignrs. retention of x-nter b y occlusion, cspecinlly w h e n cr1;st:illizctl in large grains. &-l'hc estrcinc sensitivcncss of :; fc\v or the sugars to decomposition 3.t tcriipcrnt~ires much I,clo\v 100" C., notabiy i c v ~ i o s cmid rlinmnow. ~--Thc [:let t k t such suynrs 3 s iiialtose, Inctnsc. niicl rsflinose rctxiii v:irinblc aiiiotints ol xwtcr or cryst:illizntion unrIcr diffcrcnt conditions of d r y i n g . l--Tiie
?--'f!ic
On this nccount, whether the drying is to tic acconiplisticd in tlie opcn, oncli siig:ir must be considcrcd Iry itself. I'i\,c grniiis of tlic sugar :trc acciirntcly weiglicd in a tared :iluriiiiiiuin dish, npprosim:itc.ly S.5 niin. i n di:imcCcr nnd 15 i n r i i . liigti, fitt.cd with :in nirtigiit, covcr of tlic s:iinc ni:itcri:d. l'hc w p i r niid tlisli arc plwcd i n :in c1cctric:tlly coritrollcd drying ovcn :iiitl licld for 1 lir. :it :iboiit 50" C. with propcr vcLrit,il:ition to cnrry olT t.lw moisture. Xftcr this prcliniinnry cjrying the door of tiic ovvi1 is cloec~l,tlic tcriipcrnture adjustccl to 100" C.. nnci tlic tli.ying contiiiurcl for :in :idtlitiond -1 lirs., or ovcr night. \Viien t h e sugxr i s to he removed f r o m tlic o \ w i it is seciircly covcrcri xnci transfcrrcci to thc tlesiccntor, cooled : ~ n dweighed 8 s usuni, repiaccd in t h c o w n , dried a n itdditiorinl 2 Iirs., n.&K\icd xg:tin, :md tliis inctlioti is continucd until the weight is constxnt. In tlic rnse of lcvuloec (In. p. 95" C.) and rhaninosc (m. p , 'i12.8" C.) t.iic sugar must be clried over night to const:tnt wcight a t about 5" I~elowtlic melting point. I n this Inlxnttory, wgxrs :uc clried i n large \.:LCU~RI slielf dryers for 12 to 1s Iirs., with a v w i i u m of 29 in. and running wit,cr wit11 tticrmostntic control n t not O Y C Y 120" F. We a t t e m p t to mnke the residual rncisturc nil. In the drying of invert sugar sirup and siniilxr products, thc iisual tcclinique of drying up011 washed and ignited qunrtz s:ind is observed. Fivc grains of tlie sirup are weighed accurnt,ely, dilutcd to 350 cc. in a volupctric flask, a n d 50 CY:. of this dilution t:ikcn froin the moisture assay. r xi>T: 1-t1.rI ES- 1r i t cs t i 11 :: for i ni purities , t 11 c pro cc d I i rc is as iriitlcr V R C U U I ~or ~
loilows: .4ZcuhoZ-\SVlicii I I:C. uf iodine T. S . nntl 1 cc. of potassium hydroxide T. S. UI'C :iddcd to 5 cc. of :I 20 per ccnt solution of t h e sug;tr i n divtillcd water, 110 odor of iodoform shoiild ix pcrccptiblc d t e r shaking. Chlol-idcs--\VI~cii 3 drops of dilute nitric acid ant1 10 drops of silver nitrate T . S.arc :idd(:d to 6 cc. of n 10 pcr ccnt solution of t h e sugar in tlibtilled water, :ind tlic rriistrire r~llon.~cl to st.:iiid alt,cr shaking, t.11~sugrir should SIIOM. iiot inore t h i n n vciy sliylit t~r:tccof cliloridc. zd/u~c.s-- \VI I ( J I i 3 clro 1)s o f cl il i i t r: \ i y d roclil or i c :xiI 1 :i i i 1.1 1 0 (lvops of lxiriuiii dilvritfc 1'.S . :.ire stlclcd to 6 cc. of n 10 j)cr cr.:nt S l ~ ~ l J t ~~f~ i tlic I l sugar i n clist,illwl uxtcr, tlic sugar rlroul~d sliow r i o t inore tli:rn :I \'cry sliglit tixce of su1f:ifcs. C ~ r l o i z t n z - ~ ~ ~ l i rt *o ntil(! : t i ~ o i ~solution, c tn:itlc d k d i n c with
nninioniuni hyciroxicic, :uni?ioniiim os:il:ite T S..is. :~tldett! no hnziness or turbidity should develop. Ilency Nc/ds-Whcn 2 cc. of hytirogcn sulfide T.% :irenddcd to 5 cc. of :t 10 per ccrit solution of thc sugar; :md,ttiu. inixturc hcnted, no discoloration results. :Us0 when L of hops IS added to 160 cc. of :i 10 per ceiit boilirigsolutioii ufi the s u p r 2nd the xrusture botlcd for 20 niin., no greenidi o r black color, due to iron t:inn:itc, slioulti be formed. REAumos--In testing ttic reaction of o u r sugiux, 4 IC, or,tiiw sugnr arc dissolvcd in 50 c c , of tlistilled water, 2 drops of< plicnoIplithnlein arc titided, a n d 1 drop of 0.1 .V sodiiiin hydruxidc must change the color of tlic? indicator, showing t1ie~:~i)scnce of escess &3ty. SPECIAL '1Esrs
The above tests are made on all sugnrs. In atidition.tiiem arc n fcw special cases to Le (coilsidereif. GaLuxosE-In the routine amilysis of gnlactaeie, we. t-cot: for t h e presence of buriitrn in 3 cc. of a 10 percenksgoluhot; of: t h e sugar. I?XF.RT S U C ~ Rsirzrrr-In inverb sugar- sirup, t h o detwinination of reducing surars is made' by- the DdrcnO'SuUivitn method and it shows complete cwnvcrsion. on, the. dry basis. ,\ionreducing ~ ~ i ~are a rabsent. s L.KXSE--III the :Ln:ilyis of lactose thc >ugiLr m u s t Ile f r o m nitrogcn :ind fat. I t riiutlt further show purity from ticxtrt>b.c?by two I u p t m h . tests: l-Lnck of nciriitv in culture medi:~, urirLi:r tiic itifiiicrice oB the L i . lypllo&lrJ. ?-Lack of firis formation 1x1 90 hrs.' incubation (IF 111 r x . 01.31 50 per cent solution of the sug:ir i n tlie prc~cmccor :in c\ce\s-ofi yeast.
TLWFISOSE .\SD l~H.\xfNOsE--Rltlf~iow (q5 &Ql :iIldj rhamnose (1 H J O ) :ire p u t on the mtirket :ISiiydcites. E t f f i nose is also niarketed as the anhydride. sucRosE-Suerme is tested vcry carefully irr n d u c i n g substances, nocording to the Bureau of Sk~~irlrtnIs test;" with Strieglcr's solution. Under the condition of this test;. if i o g. of sucrose in SO cc. of distilled w t a r - s r e acld~rt.tm~.St)t cc. of Strieglcr's solution (which Iins been boi1ed.l i r i i n . ) :mdt2iw mixture boiled exactly 5 niin., not; inore tlinn 0.007 .LZ (S'uiOl :ire precipitntcd. Immediately a f t e r S rnin. of kioiiing :tny possible further hydrolysis of the siicrow 15 e1iiiiin;ttcdi by. dilutinq tlic niisturc with L O O et', of c o l d , rccently boilcd,. tlistilleci w u ter. Cr~ .VLL us10 N I n contlusion it should be s t a t e d t h a t in o u r wrirk. t m i st:incl:trdizing these products, we aim a t an ult,imuh, degree. of purity t h a t will wiimint the designation of "(2: Pi" Ih our opinion, however, this dcsignntion should. be rcsemerEfarr chemicals in which present nirthods of nnaly-siswll revcal:no~ traces o f impuritiec We cannot pretend, that. them r i m sup,:m we susceptible of tliiv perfection except; by sucii, repetitions of crysttnllizatioti t h a t the yiclcl i s nlwuntly smidl\ :ind the resulting cost prohibitive. ' r h c ~ l u r c TVO rofrninl from using tlie tcrm C. P., although constantly FtrisinK f i n it. I n the present uses of tliese products, t h e niiiin,consi&w ation is tlint cucli one slid1 be frce from o t h e r csrboliydmhx This n o lire nble to nr-liiavu with an cneour:igiriE :itnounk of: Pliccc~'
If rcwirch s l i o i i l t l iiow I)c tiirixtrxl t o fintiinp t i t w I I X C fnrr the w-c:illctl xtrv b u p ~ r s ,c.1~ illy of w i n n i t m i d r i r lo% purifird gr:dc:, i t irould bc :I Krciit lif!lp to tiic d r ~ \ ~ c ~ l r i ~ ~ i of the C;. 1'. liric., d:Lhic :it .iprice t hiit I > rt~:i~cinal~lc
