Documente Academic
Documente Profesional
Documente Cultură
With the advance of science and technical ideas sugar mills have
of late years improved their methods and efficiency in almost every
direction, but in most mills no great advance has been made in t h e .
study and improvement of sugar boiling as this art was found not t o
lend itself easily t o such met,hods. Recognising the need for study
in order t o bring about the improvement of refining quality of raw
sugars, the Mackay 3Tanufacturers' Association inaugurated these
researches and this paper is submitted to the Conference through their
courtesy and generositv. At the outset a visit was paid t o the
U.S.R. Co.'s Research Laboratories and assistance rendered by this
Company was found invaluable for this work. The investigations
were carried out a t each of the seven mills in the Mackay district,
a t which i t was found that the co-operation by Xanagements and
Staff was largely responsible for the rapidity of the progress made.
BOILING.
Graining.
This most important operation, which from the outset reflects
largely upon the quality of the final grain, was first studied and i t was
found that uneven grain was due t o a great variety of causes. The
varying causes were made quite clear t o each mill by microscopic
examination, ant1 i t is pleasing t o note that they now each have a
microscope upon the pan stage in constant use. It was obvious
in most cases that the unevenness of the grain was due t o : (1) too
long a period by the waiting method for the required number of grain
t o appear : this wolxld often take as long as 20 minutes with grain
coming in all the time. with the result that the crystals which appeared
a t first were much larger than those towards the end : (2) a far worse
fault was new grain appearing throughout the skip : thus, although
a n initial uneven crop remained the same in number throughout
the boil, it would have a tendency t o even up considerably in size a t
the latter stages, ~vllereasgrain coming in all along would make far
greater unevenness. The maintenance of ~ t e a d ysteam and vacuum
conditions on the pan stage is a prime necessity for good grain, and
a recording vacuum and/or temperature gauge for the graining park
was found t o be a most vahxable guide.
Conglomerate Grain.
Dnring the early part of these investigations it was found that;
cry;ital complexes, conglomerate. or curly grain were very easily
forn~ed,t o the extent of as mueh as 80 per cent,. by weight, and this
type of grain was very difficult t o avoid under the then existing con-
60 PROCEEDINGS FIETR ANNUAL
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CONFERENCE April,-1934
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ditions (Plate 111, Figs. 26, 26, 27). This type of crystal is easily
distinguished from the aggregates of crystals, being generally formed
on twin cryatals with crystals growing from near the centre i n all
planes, and consequently star shaped when viewed on edge. Further,
as opposed t o aggregates, the crystals of true conglomerate grain
cannot be separated without breaking the crystals.
It is presumed that the refiners' objection t o conglomerate grain
is based on the syrup or molasses film which is enclosed in the very
centre of t h e crystal, and which cannot be washed away during t h e
affining process because the crystal remains complex after washing.
This condition is borne out by analysis. During grist analyses of raw
sugars i t is generally found t h a t the conglomerate grain is more con-
centrated in the larger crystals, as is seen in the following tabulated
result of a n analysis :
The figures shown under the sub-heading " conglomerate " repre-
sent the percentage of each fraction which is present as conglomerate
grain ; by deducting this proportion from the " apparent " satisfactory
grain a n arbitrary figure, " true satisfactory grain," is obtained. An
approximate figure of- total per cent. conglomerate grain is obtained
by adding the weights of conglomerate grain on each sieve fraction.
The diameters of openings in the 14, 20, 28, and 35 mesh sieves
were respectively 1.7, .83, .5, and .42 mm., while the a,verage size
.of crystals retained by these sieves was respectively 1.41, L .O, .75,
a n d . 5 mm.
Hand picking of conglomerate grain from separate sugar samples
o n the same sieve gave the following results :
(1) Well washed good filterability sugar. Ash conglomerates
(Plate 111, Figs. 232-3) 10 per cent. higher than non-con-
glomerate.
(2) Medium filterability sugar. l . l 1 mm. fraction. Ash con-
glomerate 0.27 per cent., non-conglomerates 0.21 per cent.
(Plate 111, Figs. 234-5.)
A 9 QUEENSLAND SOCIETY SUGAR CANE TPOBNOLOCISTS
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Fornation of Crops.
It was found that the best grain was made when the biggest
"shock" was introduced t o the charge a t about graining point.
Where pans were not capable of being sufficiently cleaned o u t
between skips, there was generally sufficient " soldier " grain t o make
the addition of icing or castor sugar superfluous, as the sugar added
is not considered t o be the nucleus for grain formation. It is interest-
ing t o note that the presence of any sugar crystals whatsoever prior
t o graining point gives a very good indication of the correct time
t o shock, since as shown by microscopic observation, the crystals
which were eroded sharpen up fairly suddenly a t about graining point.
NO effect was observed by varying the quality or quantity of
" shocking " sugar, although this sphere has not been closely
investigated.
6% P R O C E E D I N G S P I F T R ANNUAL CCONPEREYCE April, 1934
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Establishment of Grain.
The time between checking and establishment, or "bringing
together," is the most critical period, as i t is a t this time t h a t the
supersaturation is more likely t o show large variations, on account
of the greater rate of crystal growth and temperature variation. Once
a pan is put upon continuous liquor or s37nlp feed t,here is but little
variation in temperature, or only a very gradual variation as the
massecuite heavies up. After checking, however, the temperature
may fall as much as 4O0P., which represents a large change i n super- "
saturation and if this takes place too sudtlenly, false, uneven and
conglomerate grain is bound t o appear. Independently of the
temperature, if during "bringing together," the supematuration
is not steadily maintained by occasional drinks, false, uneven, and
conglomerate grain may also occur. So far the best improvement
has been obtained by using a recording thermometer in the graining
pan and maintaining a gradual return t o normal boiling temperat'ure
after checking, with the addition of short drinks of water every fern-
minutes ; the latter is presumed t o be a n advantage over liquor
drinks as it results in the time of bringing together being shortened.
d good example of this is seen in C'harts 2 and 3 which represent
charts obtained fur the same graining. After a little practice, t h e
sugar boiler has no difficulty in maintaining the required vscnxuas
and can produce charts of quite uniform appearance. It Inay be again
emphasised here that when using blends for graining, the eveness
or otherwise of the initial crop is by no means as irnportallt as t h e
elimination of further grain, particularly during the period of bringing
together or establishment of t h e grain.
Fig. l.-Dot diagram representing the relation between filterability and the quantit,y of
lime used for the clarification of raw sugar liquors. Data collected from experiments
at three mills.
Glaritication, Molasses Inclusion, and Pilterabilily.
I t has been found that the filterability of the raw sugar depend&
largely upon the clarification and when this process was improved
t h e filterability rose a8 is seen from the following figures:
Mill R I{
i c
6.8
6.8
6.6
6.1
7.0
9.6
7.5
6.7
very low
7.5
Mill C 6.9 5.7
Molasses Inclusion.
Molasses inclusion (impurities embedded in the grain), is
aggravated by poor clarification, and the former was found to have
a great effect upon filterability, particularly t,hat of the affined sugar,
as the impurities were not all washed away during affination. The
66
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which is crystallising out, and the different types are clearly seer1 i n
the photographs.
(4) The sugar from (3) was washed with unsaturated sugar solution
until more of the crystal tlissolved and the zone of the central
inclusion was reached. The crystals were &hen washed
with saturated sugar alcohol and dried and gaye a n analysis
of 0.13 per cent. of ash. This figure leaves no doubt as t o
the extent t o which impurities may X)e ernl~edcted in the
grain of raw sugar. (See Ylate TT., Fig. 239.)
99.98
Ratio : Internal Imyur. ---0 ' 7 1 .37
- ----
Total Impur. +
l . P2 0.71 -- 1.0
At one mill with filterabilities for raw sugar for 4 weeks as follows:---
1.8, 1.$, 2.1, 1.'7 (see Plate III., Fig. 35%),thefilterabilityfor affined
sugar was only 4.76 for a bulk sample of the above period. At a later
date with the shifting of the inclusion towards the edge of the crystal,
although the filterability of the raw sugar a t this mill wras only 1.9,
t h a t of the saturated sugar washed raw, was 9. l, so that the position
of the inclusion plays an important part in refining, the nearest t o the
centre being the worst. Figs. 513-517, Plate W., show. the character-
istics of late inclusion.
As i t appears t h a t central inclusion would be formed early in the
growth of the crystal, excessive amounts of water in the early stages
of t h e boil should be avoided, and in some instances advantageous
results were obtained by cutting down the size of the pan water supply
t o 4 t o 4" pipe. The depth and position of inclusion within the crystal
varies considerably as will be seen in the photograph. The position
i s located by focussing upon any particular surface or edge of the
inclusion, in relation t o a surface or edge of the crystal, and measur-
ing the difference. When any measurements are taken within tho
crystal. allowance is made for the refractive index of sugar. The
writer has been unable t o discover in the literature any descriptions
or photographs of inclusion, so t h a t with this paper a comprehensive
series of photographs is included,
Laboratory attempts a t reproducing inclusion showed t h a t con-
trary t o the conchisions arrived a t from factory observations, erosion
is not the cause of inclusion. I n the laboratory i t was found t h a t
circulation was the main factor as. even with eroded crystals as seed,
no inclusion was formed when the syrup was stirred during crystal
growth. With either eroded or " perfect '' seed, when the syrup was
not stirred, the crystals were found t o grow with " step " formation
(see Plate VIX., Figs. 643-618) and that with any subsequent growth
with stirring, inclusion invariably occlxrred. This step formation was
noticeable in many mill raw sugars, particularly where filterability
was not good. From the above few experiments i t would appear
t h a t the best defence against inclusion is (1) good clarification with
resultant decrease in impurities and s~iscosity: (2) good circulation
and uniform boiling conditions. On this account intermittent feed,
with its resulting sudden changes in viscosity and circulation, should
be avoided, as also should sudden variations in steam or vacuum.
Magma System.
The investrigation in Mackay has shown cleax-ly the advantage8
of nsing magma seed, in the eyennesa of the grain, and the saving
68 PROCEEDINGS BIBTH ANNUAL CONFERENCE
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April, 1934
grain in the screw or pump wa* founcl t o inflllence thc yaality of the
final grain (see Plate IT, Figs. 96-8) ancl consequently this should be
avoidetl as far as possible. As the grain size of individual C's will vary,
keeping the magma separate will assist in maintaining unifornl grain.
instruments for Gontrol of Sugar Boiling.
Owing t o trhe pressure of other work, not much time was devoted
t o these instruncnts, but the following ronclusions may be of interest:-
Eleetrieal conductivity apparatus.-An instrument similar t o
the Cuitorneter (Xntcrnat. Sugar Journal, F. Todt. Feb. 1933, $ W. F,
Alewjin, Sept).1938) \v88 tried on a graining pan but probably oning
t o variations of temperature and purity, consistent conctuetivities were
not obtained for graining point, so t h a t the results t o date show n o
superiority over the judgment of the sugar boiler. The simplicity
ancl low cost of this instrument. however, merit further study for i t s
application for boiling control.
Temperatnre Difference Recorder (Smith, Faet* about Sugar.
Feb. & March, 1932).-Two different makes of instrnment, Leecls,
Northnipp & C'arnbridge, were studied when in nse with c*alandria
pans for high grade sugars (A & AB). Althougll insufficient data
have been collected t o enable the construction of ideal curve# for dif-
ferent types of massecuites (o>$-ingprobably t o variation of purity
a11tl temperat~xres.size of seed grain,etc.) the writer belieres that the
use of this type of instrument is of great assistance for (1) minirnisiilg
the percentage of fine grain : and ( 2 ) recorcting the method of boiling
each strike and the ps~chologicaleffect of improving the work of t h e
sugar boiler, as well as being a gootl guide.
Explanation of PhcitomirvograpIi8.
Figs. 381-387. Four skips A Sugar from graining chargr; 1XlM) Lquor: 7tM) AB
Syrup.
Figs. 37$-375. Four s k i p d Sugar froln prainlng (har<e; 1700 Liquor; SO0 -%B
Syrnp. Theqr J t i p mere made simulta~~eously
a t the Lame 111111.
Fig. 215. 17ina1 AB massecuite from nmglna. Bad tlrier.
Fig. 236. Final B inassecuite. Bad <trier, ex graining.
Fig. 2 i i . Final C' nia-rruitr. Bad tlrirr.
Figs. "$6-"57. Blrntl 85.8 apparent purity for (' shock w d e d Brcwcr.;' C'ry.+~ls.
1-aruum maint,ainecl 23" vhilst bringing toget,ller n i t h short
drinks of water.
Fipa. 216. 'l minutes after c.hecBing ; 24'7, 12 minutes :
Figs. 21% 41 minutes ; 250, I lrour 10 minutrs ; 3.51, 1 hour 1.5 mirxtc..; ;
232, l hour 20 minutes on to continuous B syrup feed :
257, (! u~aaswriit~ from above 64 Ilourd after (:heck-- ptm haif
fllll.
Coorl grcrirti~cy with w i t i r r g v i i t l ( d . Blind. Graining blend app. purity 80. By wait,.
ing mc~thorlgrain rame in w r y small and eve11 ; x-cr>-gradual tlro~)v a c m ~ X-lrm l
bringing together: S C P charts 1 ant1 2.
Fig. 516. " 0 minute; after cliecl;.
Fig. 519. 3 hours; R". ('at to ( ' JI;U: 3 8 Ilonv.;.
.Tip. 25, 26, 27. ('onglomrmtc grain. Hlen l . \-aristion; ttwpi.ratirr~~aft:.~ d w k -
ing too sudden.
Fig. 231. 1.11 mm. sieve frartion, &ABsugar ;iortt,tl single crj-stab ; a& I!.21 cwt.
Fig. 293. A masiec.uitc2 drying ~rt'll. Sa~nplefrom ncur fugal g,r~ugv. S ~ ~ n fine
w
pail].
Fig. 2514. S:nr~e as 293. From midtllr of s a p r l i ~ y e r : nnifiirli..
Fig. 613. Smlc as 612, 0 . 1 inm. focos below front oi.tllol)irinc~oiti: tilt. sitlnc! a i
612, ffoeur;0 . k n m . helow left p l c ; 613, sanle as 612. few- 0 . 1 rnrn.
kelow l m a l liinncoitl. Indirates different rat(, of growth ia different
clirrctio116.
Fig. 590. Stale cane----magnln--.1attt I w a l pinarwid inchtsion.
Too rarltleu drop t ~ m p r m t u r cafter checliinp ; graining.
Magnlu ~ o o ( llittle
. fine grain.
Fi11e grain front a b o w " clean u p " in pan.
H ntassccuite from above, 2 llours l a k ; abwnre of fine grain
U marise~~oitrfrom el)orr, 3 hours later; ahsence of fine p i n , little
light inclusion.
Bad magma, uneven and with in~lusion.
massecuit,e from abow. Very uneven con,rrlomevate and full of
inclusion.
(! nugar 9.5 nngnia from a l m ~ c .Morca fine grain owing to magma w r r w .
; 96 C> sugar from above ; 98 magma from ahovc ; more
C' rnasseruitc
fine grain o~vingmagma wrev.
Good even magma fwe from fine grain.
Xt~grna,inc4asion ant1 fine grain. 240 reed fro111 ahtrrcx not effectiroly
cleaned up.
Final A masxecuite (1st cnt) front above showing unrvennrxs. 21;.
Final -4 rrmsmwite from almrc more e r m , inor? irtclu-;ion (,%cl ?cut),.
- 78 PEOCEEDTNGs FIFTH ANKUAT. C'OKFERENCE d j ~ i ? 1934
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['l. *Tr T .
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Explanation of Photomicrograph*
Pig. 368. Seed for (', shock blend. 2 l i o u r ~after cllecli ; indusioxi due to exce*,
water and eroJion of gram 111 attcmpting to remore false grain.
Pig. l . Inclus~onin jelly " sugar; no water used.
"
Fig. 372.
Fig. 379. Sxnlc~a.: :iW, focwsed 0 . 1 6 trim. bc~lowfront ortho pinaroid ; depth or
c r ~ h t a l0 . 6 mm. Not(, qteppetl fornlation on edge of crystal.
Fig. 434. Induclon in jrlly hugar, uiore niarketl in larger rr~atalh.
Fig. 1.54.
Pig. 4.55. Same as 451, focus 0.1.5 nnn. Ijelo\\-front ort,ho pintacoicl ; note " jagged ''
inclusion.
Fig. 4.56. Same as 455. f o c w 0 . 2 3 mm. brlow top hasid pinac.oirl. (Total depth
0.4ti nnu.)
Fig. 4,55. S a n ~ ca:: $56, foews top hasal pinacoid.
Fig. 513. Tvpival rr?.stals with right pole inclusion ; filterability 3 . R.
rip. 311.
Fig. ,51,5.
Fie. 516. Same as 31.5, f o ~ ~ u s w bt4on
l top I)t~.;olpinacoitl. Inclusion co~lfinad
to right pole. gettint?.hravier towards tlic cntl of a boil.
FIR. -517. Same R:: 516, f o c ~ ~ x ~front
r r l p l c face and showing pitted t u b n l ; ~etching
of surfac,i,.
F1g. :3im. I3 ;jug;rt from Mill "A" for week c~ncliug7th Ortnhrr. 1!)33 ; 0 . 6 filters-
bility. ltravy inchwion.
P1p. 507. K sugar from Mill " A " for \r-t'~li ending 2nd I)rccnll:er, 1!1:3:3 ; 7.1
filtershiliby ; inciunion orlly in trawx.
J ' L A ~ VJI
-- --
.
Explanation of Photomicrographq.
Fig. 543. Sifted fine grain used t o seed saturat,ed AI3 syrup a t 158' F., stirred nnt,il
cold and viscous, no t:irculation. 18 % .
Fig. 514. 9%543 ; crystals gre,w normally lintid a t end of stirring, no circnlat,ion
on stanging, late right pole inclusion. 1 8 ~ .
Pig. 545. Same as ,544, fihoning one very irregular " ~ t e p p c d" cryst,al. IS:.'.
This formation obt,ainal~leunder any condit,ion of parity, t'emper-
atmureor rate of crystallization, providing no circulation ohtaina.
Fig. 546. 544 used t o seed fresh sample hot AI3 syrup. Crystals grew normally
during stirring : late inclusion 01 541 now appears
~. nu early inchwion.
18x.
Pig. 547. Graded twins, some with early inclusion used t o seed saturated AB syrup
a t 15XcF.; did not grow much owing t,o fiue grain crop bnt stepped
forma,tion occurred. 18 X .
Fig. 548. RC& 547 ; stepped " twins, used to seed further sample AB syrup, grew
"
I'L~TE \.It.