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Sugar and Other Sweeteners - Handbook of Industrial Chemistry and Biotechnology-Springer (2017) PDF
Sugar and Other Sweeteners - Handbook of Industrial Chemistry and Biotechnology-Springer (2017) PDF
Abstract
Sugar and starch are among the most abundant plant products available,
and large industries exist worldwide to extract and process them from
agricultural sources. The world production of sugar (sucrose from sugar-
cane and sugar beet) in 2015/2016 was approximately 176 million metric
tons, raw value, with 19.6% being beet sugar and 80.4% cane sugar
(Supplement to A first look at the 2016-17 sugar balance, 38, 2016).
The total production of world sugar has risen dramatically since 1971/
1972, when it was 71.7 million tons (FO Licht GmbH, World beet and
cane sugar production, 14–15, 2004). The proportion of beet sugar to cane
sugar has fallen steadily since about 1971, when it constituted 42.8% of
total sugar production (FO Licht GmbH, World production, consumption
and stocks of centrifugal sugar 1952–2000, 12–13, 2001). In 2015/2016,
37% (66.0 million metric tons) of world sugar production was exported,
with Brazil being the largest exporter (Supplement to A first look at the
2016-17 sugar balance, 38, 2016). China was the largest importer in 2015/
2016 followed closely by Indonesia, the European Union, then the USA
(Supplement to A first look at the 2016-17 sugar balance, 38, 2016).
Although, in some developed countries, there is currently an unhealthy
perception of sugar with associated campaigns to reduce sugar calories in
foods, world sugar consumption continues to climb. World sugar con-
sumption was 182 million metric tons, raw value in 2015/2016, due
mostly to Asia, Africa, and North and Central America (Supplement to
G. Eggleston (*)
USDA-ARS-Southern Regional Research Center,
New Orleans, LA 70124, USA
e-mail: gillian.eggleston@ars.usda.gov
B. Legendre
Audubon Sugar Institute, Louisiana State University,
St. Gabriel, LA 70776, USA
M.A. Godshall
Metairie, LA, USA
A first look at the 2016-17 sugar balance, 38, 2016). Per capita consump-
tion of sugar in 2015/2016 was greatest in South America (51.3 kg, raw
value) and lowest in Africa (17.8 kg, raw value).
Keywords
Sugar Manufacturing • Juice clarification • Evaporation • Sugar Refining
and Purification • Decolorizing and Packaging • Sugar Recovery from
Molasses • Sucrochemistry • Other Natural Sweeteners • Regulation and
Trade • Genetic Engineering
of starch as a source of nutritive sweeteners [5]. - units. The vacuum pan appeared in 1813, bag
Starch-derived sweeteners have competed filters in 1824, multiple-effect evaporators in
directly and successfully with sugar in the United 1846, filter presses in 1850, centrifugals in
States, but in recent years their consumption, 1867, dryers in 1878, and packaging machines
particularly high fructose corn syrup (HFCS), in 1891 [13]. Cultivation of the sugar beet plant
has declined. The latter is mainly due to multiple and the manufacture of sugar from the beet
consumer issues, including high fructose content, developed in the industrial nations of Europe
GMO, and links with obesity and medical during the eighteenth and nineteenth centuries.
diseases such as diabetes [6]. In 1747, the German chemist, Marggraf,
The sugar industry is a mature industry and established that sugar from beets was the same
thus typically characterized by steady, small as sugar from cane. His pupil, Achard, in 1799,
incremental improvements in technology and demonstrated that sugar can be commercially
production over the years, with subsequent prepared from beets. During the Napoleonic
improvements across the process, from field wars, a short-lived beet sugar industry was
practices to new products [7, 8]. established in France [14]. Today, beet is the
major source of sugar in Europe.
Sugar Manufacture
Raw Sugar Production from Sugarcane
History [9]
Traditionally, raw sugar is produced at the sugar-
The ancestry of sugarcane and its use as a food cane factory and white, refined sugar is produced
have been traced to the island of New Guinea. at a refinery, often far removed from the source of
Around 8000 BC, the plant started on its migra- the raw sugar, and close to areas of consumption.
tion from New Guinea to many areas of south- Figure 1 is a generalized flow scheme for the
eastern Asia, Indonesia, the Philippines, Malay, manufacture of raw sugar. In summary, juice is
Indochina, and eastern India, with humans most extracted from the harvested cane stalks, and the
likely acting as its main dispersal agent [10]. Sug- juice is clarified, concentrated by vacuum evapo-
arcane was first cultivated in Bengalese India as a ration, crystallized, and centrifuged. The several
field crop and the juice manufactured into vari- steps are described in the sections that follow.
ous solid forms. A general knowledge of sugar
was prevalent throughout India by 500 BC Agriculture. The sugarcane is a large perennial
[11]. By the tenth century AD, sugar cultivation tropical grass belonging to the genus Saccharum.
and manufacturing had become important Three basic species, S. officinarum, S. robustum,
industries in Persia and Egypt. The early Islamic and S. spontaneum, make up the sugarcane com-
movement spread knowledge of the sugar indus- plex, with a large number of varieties. Sugarcane
try throughout the Mediterranean area. On the is propagated commercially by cuttings, each
second voyage of Columbus to America, in cutting consisting of portions of the cane plant
1493, sugarcane was introduced in Santo having two or more buds, or “eyes.” The buds
Domingo. It spread rapidly through the West sprout into shoots from which several other
Indies and Central America. Cortez brought shoots arise below the soil level to form a
cane to Mexico, and Pizarro introduced it in clump of stalks known as a “stool.” From 12 to
Peru. By 1600, the sugar industry was the largest 20 months are required for the crop to mature
industry in tropical America [12]. from new plantings and about 12 months for
The modern sugar industry dates from the end ratoon crops (i.e., cane stalks arising from stools
of the eighteenth century, when steam replaced that have been previously harvested). However,
animal energy and made possible the develop- in subtropical areas, i.e.,Louisiana, USA, sugar-
ment of larger and more efficient production cane is harvested at 7–10 months because of
936 G. Eggleston et al.
imbibition water
Raw
Bagasse Sugar
Centrifugation
Molasses
Fig. 1 Basic flow scheme of the manufacture of raw sugar in a sugarcane factory (from [15])
freezing conditions during the harvest season. taller. The cane stalk is round and jointed, and
Most of the field operations have been grows to more than 3.05 m when mature (Fig. 3).
mechanized, but planting is still done by hand It is covered with a hard rind that varies in color
in some cane-producing areas (Fig. 2). Fields are from light brown, green, yellowish green, purple,
replanted after ~2 to 5 or more ratoons (cuttings or striped, depending on the variety. There is
made from the original planting), depending on usually a fine film of waxy material on the sur-
the country. face of the rind, heavier in some varieties than
As cane grows, its foliage is largely limited to others. The stalk is divided into a series of
the upper one-third of the plant, as the lower internodes, from 7.6 to 25.4 cm in length,
leaves senesce from shading as the stalk grows separated by nodes. The internodes contain the
Sugar and Other Sweeteners 937
bacteria consume the sugar, and in the produc- chopper and the shredder into a single unit
tion of undesirable by-products, such as dextran, [20]. The advantages gained are a greater
mannitol, and lactic acid, which are discussed in increase in juice extraction by the mills, an
a later section. increase in the grinding rate, and, in some
The cane is prepared for milling by mechani- cases, a decrease in power consumption by the
cally knifing or shredding or a combination of the milling operation. The preparation index (PI) is a
two to chop the cane into smaller pieces. It is measure of how well the cane has been prepared
important for the mill to pay attention to good for juice extraction, and represents the percent-
cane preparation, in as much as this is one of the age of cane plant cells that are ruptured by the
most important parameters affecting extraction cane preparation equipment. It is measured as
of the juice [19]. The Unigator, developed in Brix (percent soluble solids) in the ruptured
the late 1970s, combines the action of the cells as a proportion of the total Brix in the cane.
Sugar and Other Sweeteners 939
maximum expression of juice. Diffusers have Biocides. Biocides, briefly mentioned above, are
capacities ranging from 200 to 500 t of cane per chemical substances used to control microbial
hour (newer ones have capacities up to 875 t/h) contamination during industrial processing, and
and may be used alone or in conjunction with are important in both sugar beet and sugarcane
part of a milling tandem, the crusher, and the first processing. Biocides are usually a type of pesti-
mill. Preparation of the cane for diffusion is cide (fungicide, algicide, insecticide, etc.), or an
essential for good extraction. In the diffuser, the antimicrobial (antibacterial, antibiotic, etc.), or
shredded cane is countercurrently washed with both. During sugarcane and sugar beet processing,
imbibition water at an average temperature of favorable conditions in temperature, juice pH,
~80 C. The high temperature helps to prevent water activity, sugar and nutrient content promote
microbial growth in the cane juice, but also microbial growth, resulting in sugar loss
increases the color of the juice. The last stage [25]. Biocides reduce sugar loss by slowing
of a diffuser, the bagasse exit, receives water that microbial growth (bacteriostatic) or killing the
gradually increases in sugar content as it pro- microorganism (bactericidal). Examples of bacte-
ceeds to the final stage. Most of the sugar is ricidal compounds are sodium hypochlorite,
extracted in the first four or five stages by simple hydrogen peroxide, ozone, glutaraldehyde, and
displacement of sucrose from the ruptured cane quaternary ammonium compounds, i.e., ammo-
cells. In later stages, diffusion occurs in nium bisulfate and benzyl ammonium chloride
unruptured cane cells. At the end of the diffusion [26]. However, hydrogen peroxide and ozone
process, there are one or two mills to express can cause high acidity and acid degradation of
water from the discharged bagasse sugars. Thus, they are usually added with lime.
[21]. Chainless diffusers were introduced by Other compounds like dithiocarbamates, hops
Bosch Projects in 2006. The chainless diffuser acids, and rosin acids are classified as bacterio-
eliminates the need for chains to move the cane, static, which limit growth. In the United States,
consisting instead of modules that move indepen- sugarcane and sugar beet factories are regulated
dently, actuated by hydraulic cylinders [22]. by the Food and Drug Administration (FDA) and
Diffusers, compared to tandem milling, give are allowed to use dicarbamates at < 4.1 ppm,
greater sucrose extraction (up to 98% dimethyl benzyl ammonium chloride at <
vs. 92–96% across a tandem mill), but with 0.68 ppm, and glutaraldehyde < 250 ppm. Due
greater impurities extracted [23]. Diffusion to regulations and availability, the biocides most
provides a clearer juice (due to the filtering effect commonly use around the world are dithio-
of the bagasse mat) with lower starch and gums carbamates, glutaraldehyde, and ammonium
but with ~25% higher color. Operation and main- bisulfite. Combinations of these biocides may act
tenance of diffusers is typically simpler than for synergistically [27]. The use of natural products as
tandem mills, but the initial capital cost is higher. antimicrobials has received attention in recent
Also, diffusers have low power requirements years, and most natural products are unregulated.
since low-pressure steam can be used for heating Hop acids, rosin acids, and palm kernel fatty
in the diffuser and because of their typical acids, especially myristic acid, have shown prom-
enclosed and insulated system which offers ise [28, 29]. The recommended use of both
good heat economy. During diffusion, less filter synthetics and natural biocides is mixtures and
cake is produced than for tandem mills because rotations to prevent adaptation by
its mat of shredded cane acts as a primary filter microorganisms. Natural biocides have the advan-
[23, 24]. Cane diffusers have been installed in tage of being biodegradable, less toxic and can be
sugarcane factories throughout the world and are used in human food. Additionally, myristic acid is
manufactured by a number of companies. Many precipitated by lime during clarification [29].
large sugarcane factories have diffusers, the
major exception being in the United States, Dextran and mannitol. The major
where only one factory has a diffuser. microbiological losses in sugar processing are
Sugar and Other Sweeteners 941
Fig. 7 Production of
metabolites (degradation
products) after a sugar juice
was infected with
Leuconostoc mesenteroides
bacteria. From [30]
penalty for high starch concentrations in raw (35–40 C) in tanks with retention times up to
sugars. Insoluble starch that is not totally 12 min [42]. The limed juice is then pumped
solubilized during the factory clarification pro- through heaters, then flash heated at ~102 C to
cess persists into syrups, massecuites, molasses, remove unwanted bubbles. Many modifications
raw sugars, and even refined sugars [36– to this process exist, especially with respect to
38]. Insoluble starch can interfere with viscosity the heating of the juice. Fractional liming with
[36], filtration [39], and applications of double heating involves liming the cold juice to
α-amylases to control starch. Most methods to pH 6.4, heating, liming to ~pH 7.3, and then flash
measure starch in the sugar industry only mea- heating and flocculant addition before sending
sure total starch. Only the USDA research the juice to the clarifiers. Flocculants, typically
method [37] is able to measure total, soluble, high molecular weight polyanionic acrylamide
and insoluble starch. flocculants, are added to agglomerate particles
and add weight to the calcium phosphate flocs.
Juice clarification. The sugarcane mixed juice Because there is no pre-heating of juice during
obtained from milling or diffusion is acidic color lime clarification, the flocs are small and
(pH around 5.4–5.7), turbid, and dark brown in settling is relatively slow and inefficient. Further-
color. It contains 12–18% by weight sucrose more, dextran forms in the lime tanks, erratic pH,
(depending on the maturity of the cane), in addi- color, and turbidity control occurs, and consider-
tion to soluble and insoluble impurities, such as able sucrose losses can occur [41, 42] (Table 1).
soil, protein, waxes, polysaccharides, insoluble
starch, fine bagasse (bagacillo), organic and phe- Intermediate temperature lime clarification. This
nolic acids, soluble salts, and water insoluble is similar to cold lime clarification except that the
pigments. Sugarcane juice also contains from juice (only 30% needs to be heated to gain
0.5 to 3% reducing sugars (glucose and fructose benefits [41]) is pre-heated to 82–93 C before
in approximately equal quantities). Juice liming in a lime tank (retention time up to
clarification or defecation is designed to remove 12 min), then flash heating, flocculant addition,
the maximum amount of turbid particles, and and settling in the clarification tank. Pre-heating
usually employs heat, lime, and flocculants. The of the juice creates natural flocs through coagu-
degree of clarification has a great impact on lation of colloids. Heating is also an
boiling house operations, sugar yield, and refin- excellent disinfectant and can remove up to
ing quality of raw sugar [40–42]. It can also 99.9% of microorganisms in juice [25]. The addi-
affect the juice filterability, evaporator scale tion of lime then creates larger flocs with calcium
composition and amount, and sucrose phosphate bridging. These larger flocs settle
crystallization [40]. faster and removed more turbid particles. How-
There are various lime clarification systems, ever, as lime is added to the juice when it is warm
with hot and intermediate temperature liming the rather than hot and, because of relatively high
most common. For all systems, hydrated lime in liming retention times, excess lime is still added
the form of a slurry (milk of lime MOL) or lime during intermediate lime clarification [41, 42]
saccharate solution [43] is added to the juice to (Table 1).
raise the pH to ~7.3 for (a) neutralization of acids
to minimize sucrose losses from acid degradation Hot lime clarification. This is the most com-
of sucrose, and (b) to react with inorganic phos- monly utilized clarification process in the USA
phate present in the cane juice to form a calcium and worldwide. Like for intermediate tempera-
phosphate flocs, and (c) to introduce positively ture lime clarification, the juice is pre-heated, but
charged particles to the solution (Fig. 8). The during hot liming the juice heating temperature is
main sugarcane juice clarification systems are: 93 C, and all the juice is pre-heated. Lime is
added to the hot juice for only 0.5–1.0 min,
Cold lime clarification. Lime usually in the form which reduces the amount of lime required. It
of milk of lime is added to the cold juice also has the added advantage of efficiently
Sugar and Other Sweeteners 943
Table 1 Comparison of the three main clarification processes used to purify sugarcane juice in a factory
Intermediate temperature lime
Cold lime clarification clarification Hot lime clarification
Advantages Disadvantages Advantages Disadvantages Advantages Disadvantages
Simple Color formation (~10%) Color removal good Extra juice Least sugar Extra juice
on liming heating losses heating
needed needed
Traditional High sucrose losses High turbidity Excessive Fast settling Requires high
removal (only 30% lime use temperature
of juice needs to be pH electrodes
pre-heated [41])
Least Excessive lime use Starch and dextran High turbidity
expensive removal on removal
operation pre-heating juices
(no heating)
Most erratic pH, color, Fast settling Some dextran
and turbidity control removal
Small flocs Largest flocs Very little or no
measurable
color formation
Least turbidity removal Clarified juice:
low color and
turbidity, with
good control
Clarified juice: high Less heater
color and turbidity scaling and
better heat
transfer
Dextran formation in
lime tanks
Mostly from [42]
controlling pH and sucrose losses. Lime can be clarification depends on the formation of a stable
added before or after flash heating. The mecha- flocculent precipitate which settles rapidly, juices
nism for hot lime clarification of sugarcane juice low in natural phosphates (less than 300 ppm
is illustrated in Fig. 9. The summarized P2O5 on juice solids) tend to be difficult to clarify.
advantages and disadvantages of the three main Thus, phosphate may need to be added. Very fine
juice clarification processes are listed in Table 1. silty soil carried in from the field may also inter-
Settling of flocs occurs in continuous closed- fere with clarification. The main changes in
tray clarification tanks. The settled mud after clarifiers over the last 20 years have been the
juice clarification consists mostly of insoluble development of the trayless SRI-type clarifier,
lime salts, coagulated protein, and entrapped col- which can handle much higher throughputs than
loidal and suspended matter (approximately 5% the older-type clarifiers [44], as well as clarifiers
solid matter). The clarified juice leaving the with turbulence reduction devices [45].
clarification tank is a clear yellow/brown liquid.
Entrained sugar is recovered from the mud by Syrup clarification. In some factories, a process
means of rotary vacuum filters equipped with a known as syrup clarification is used to produce a
perforated metallic screen cloth. The turbid fil- higher-quality raw sugar, in particular lower
trate juice is returned to the clarification system, suspended solids and color, as well as better
and the press cake or filter mud is usually sent to yield. It is often used in the production of raw
the fields as fertilizer. Since efficient juice sugars for direct consumption. Evaporator syrup
944 G. Eggleston et al.
Fig. 9 Schematic - -
cane juice - adsorbed colloidal
- - -- - - -
mechanism for hot lime particle -
- - - - - - particles, i.e.,
clarification of sugarcane - - proteins, polysaccharides
-
juice. Only 30% of the
Heat
juice needs to be heated to
gain enough flocs for coagulated -
-
- - -
- -- -- -
clarification [41]. A lime colloids
saccharate solution - - Heated Floc
-
provides a higher -
proportion of free calcium Lime + phosphate in juice
ions for the formation of calcium Ca2+
PO4
3- Ca2+ Ca2+
calcium phosphate flocs phosphate forms -
- - -
- - --
than a milk of lime
Ca2+ Ca2+ - - Calcium
suspension. From [43] -
Ca2+ Ca 2+ Ca2+ 3-
Ca2+ Phosphate
PO4
- Bridging
- - 2+ - - -
- -
- -- - -
Ca 2+ Ca Ca2+
- -- -
- - -
- Ca2+ - Ca 2+
- -
flocculant larger flocs
added
is treated with phosphoric acid, lime, and a poly- sulfitation is not generally used in the manufac-
mer flocculent with a strong basic cationic center ture of raw sugar which is produced for export to
(15–30 ppm). The floc contains air bubbles and refineries. Sulfur dioxide gas is mostly produced
solid particles which are held together by the by burning (363 C) elemental sulfur in a fur-
flocculant [46]. Insoluble impurities floated to nace. Alternatively, liquid anhydrous SO2 can be
the surface of the syrup and are removed by used and eliminates the need for a furnace. Fur-
skimming. Color removal (up to 10%) is not as thermore, the use of liquid SO2 has been shown
good as turbidity removal [46], but bagacillo to have advantages over the gas, especially in a
particle removal is efficient. The clarified syrup significant reduction in gas consumption (up to
goes to the vacuum pan for crystallization. Syrup 69%) and a better quality of product [48]. Typi-
clarification reduces the color and turbidity of the cally, lime (about 0.2% on juice) is added to
sugar produced, and can also be used in conjunc- reduce acid degradation reactions, with the sul-
tion with sulfitation to produce an off-white, fite ion being stable between pH 7.8 and 8.7
edible sugar [47]. [49, 50]. Many of the complex and little under-
stood reactions that produce color in cane juice
Sulfitation. Sulfitation (alternate spelling, are inhibited by the presence of SO2 gas. For
sulphitation) is the practice of adding sulfur diox- example, enzymes responsible for the enzymatic
ide (SO2), a bleaching gas, to cane juice and/or browning reaction are inhibited, and reducing
syrup for the purpose of color control. In many sugars (glucose and fructose) are blocked by
parts of the world, particularly developing sulfur addition at the aldehyde group and cannot
countries, sulfur dioxide is used to process cane react with amino acids to form browning
juice into a semi-refined white sugar, known as polymers in the Maillard reaction. The sulfitation
plantation sugar or mill white sugar, used for effect is temporary, and is better at suppressing
domestic consumption (see the section “Direct color formation than reducing it [51].
Consumption Sugars”). Sulfitation is not used in Double sulfitation is practiced in many mills
US sugarcane factories because high sulfite in in India and China. In this process, a second
raw sugar is considered carcinogenic. Moreover, dosage of sulfite and lime is added to the
Sugar and Other Sweeteners 945
evaporator syrup at a solids content of 55–65% range of 1.5–3 m in length. The Kestner evapo-
[48]. Double sulfitation provides a better quality rator consists of numerous long vertical tubes,
white sugar. 6–7.5 m long, inside a cylindrical shell. In both,
There are many variations for the addition of the juice to be concentrated is fed to the bottom
SO2 to juice, based on temperature, order of addi- of the tubes and heated, causing the juice to boil
tion, and pH levels. These include liming first, and rise through the tubes. At the top,
sulfiting first, simultaneous addition of lime and concentrated juice and vapor are separated in
sulfite, and fractional procedures, as well as separators. The Kestner evaporator has a short
sulfiting cold or hot or stepwise heating of juice. residence time and a high heat transfer coeffi-
The advantage of using SO2 is a much lower color cient, but is more subject to scale deposits.
in the produced sugar. Disadvantages include The Roberts evaporator does not have a juice/
increased scaling problems in the evaporators, vapor separator.
high sulfite content in the final product, higher Newer types of evaporators are the falling film
sugar loss due to lower pH, and secondary color tubular evaporator and the plate evaporator, either
formation (color return) on storage. Overall, there rising film or falling film configuration. The falling
has been a trend to decrease the use of SO2 in the film tubular evaporators have long tubes, like the
cane sugar industry in favor of alternative color Kestner, but the juice is fed at the top and flows
control methods, such as reducing the amount of down the tube wall as a thin film, resulting in higher
trash (leaves and tops processed), polyaluminum heat transfer coefficients and reduced contact
coagulants, hydrogen peroxide, and powdered times. However, the tubes require feeding equal
activated carbon. quantities of juice and must be kept wet at all times,
as even a short time without adequate wetting can
Evaporation. The clarified juice (about 85% lead to severe fouling. Advances and innovations
water) is pumped to evaporators where it is in evaporation are driven by the need for energy
concentrated to a syrup containing about 65% efficiency and to improve heat transfer
soluble solids. Evaporation is undertaken in coefficients. The goal in evaporation is to move
multiple-effect evaporators to achieve maximum the liquid through as quickly as possible at the
steam economy. Each effect is arranged in series highest temperature without causing degradation
and operated so that each succeeding one operates of the sucrose. The newest of the evaporators is the
under a higher vacuum (lower pressure). This falling film plate evaporator (e.g., Balcke–Dür,
arrangement allows the juice to be drawn from Niro, Inc., GEA Ecoflex GmbH), the first one
one vessel to the next and permits it to boil at being installed in 1992. Recently, technology has
progressively lower temperatures. The become available that allows the retrofitting of
concentrated juice (final evaporator syrup) is existing Robert evaporators with falling film plate
removed from the last effect by a pump. Triple-, packs and some peripheral equipment, allowing
quadruple-, and quintuple-effect evaporators are the total steam demand of a cane sugar factory to
used, occurring in some factories in parallel, with be decreased by almost 30% on cane [53]. Plate
the quadruple-effect type plus one to two evaporators are more common in the beet industry.
pre-evaporators being a common configuration.
In a four-effect (quadruple) evaporator, 1 lb. of Evaporator scaling. A severe problem in cane
steam evaporates 4 lb. of water. sugar processing is the deposition of scale on
Several types of evaporators exist [52]. The the evaporator tubes or plates. Scale deposits
older, more traditional, evaporators are the consist of calcium and silicate salts, enmeshed
Roberts and the Kestner, both rising film, tubular in a matrix of organic material that can accumu-
evaporators. The Roberts, first introduced in the late very rapidly, causing a severe drop-off in
1800s, is known as a short tube, natural circula- heat transfer and efficiency of evaporation
tion, vertical tube evaporator. The tubes, inside [54, 55]. Cane factories are forced to clean their
which the evaporation takes place, are in the evaporators on the order of every 10–15 days,
946 G. Eggleston et al.
using mixtures of acid and alkali and mechanical It should be noted that batch pans are still
cleaning. Various anti-scalants are available, required for the production of high-quality
with some, though not a great deal, of efficacy. refined sugar. One version of the continuous vac-
Evaporator scaling is a problem in cane sugar uum pan is a horizontal cylinder with
refining and beet sugar production as well, but compartments in its lower part. The pan is
not to the extent that it is in raw sugar production. provided with an additional evaporator called
Good control of clarification will help to mini- the concentrator, where the density of the syrup
mize evaporator scale. is raised to 78–80 Brix (% dissolved refractomet-
ric or soluble solids).
Crystallization. The final evaporator syrup is Seed is added in the first compartment, and
pumped to a vacuum pan, in which it is the resulting massecuite moves progressively
evaporated to supersaturation to cause sugar through the compartments of the pan. Additional
crystallization. The vacuum pan is a single-effect syrup is added to each compartment to control
evaporator designed to handle viscous materials. the fluidity of the massecuite. Approximately
It is a vertical cylinder with its bottom designed 20% of the syrup is introduced at the concentra-
to allow easy removal of the crystallized mass. tor, and 80% of the syrup is fed to the various
The heating elements used in vacuum pans either compartments through special feed headers.
are short, large-diameter vertical tubes (calandria The crystallization of sucrose in vacuum pans
pans) or coil around the inner surface of the is called “sugar boiling” and each boiling is
truncated cone of the pan (coil pans). A typical termed a “strike.” Because a single crystalliza-
vacuum pan, with a “catchall” or entrainment tion does not recover all the sucrose from the
separator for separating syrup from vapors, syrup, mother liquor from a strike is recycled
measures approximately 7.6 m in height and for recovery of additional sugar. Various crystal-
4.6 m in diameter. The working capacity is lization schemes exist to suit the purity of the
about 28.3 m3 of massecuite (mixture of crystals incoming syrup and quality of the raw sugar
and syrup or mother liquor). The shape of the pan produced. The four major crystallization
and the positioning of the heating elements schemes are: (a) Two-boiling scheme,
within the pan are important design factors in (b) Three-boiling scheme, (c) Double magma
maintaining good circulation of the massecuite. scheme, and (d) VHP (very high pol) scheme.
For example, floating calandrias (calandria not The choice of boiling scheme affects both the
attached to the shell of the pan), horizontal pans, total massecuite flows and energy required for
and pans having mechanical circulators are used. crystallization. A three-boiling system is still the
The process of crystallization is called boiling or most popular. Practically, rigid adherence to a
pan boiling in the industry. crystallization scheme all season is rarely possi-
The move toward continuous processing has ble, and some flexibility is needed to cope with
resulted in the development of continuous vac- variations in syrup quality and purity. In general,
uum pans, low-grade continuous pan boiling is overheating and recirculation of impurities cause
well established [56], and raw sugar boiling with color formation and enhance color transfer to the
continuous pans is increasing as well. The crystals. The strikes are designated by letters.
benefits of continuous pan boiling include con- Thus, the first, highest purity, strike is the A
trol simplicity, improved product quality, low boiling, and the products of the A massecuite
product losses, steam savings, steadier demand, after centrifugation are A sugar and A molasses.
and energy savings [57]. Most continuous pans The second is B followed by C. The boiling
are a variation of the original 1931 Werkspoor schemes are based on “purity,” the amount of
patent, of a horizontal cylindrical pan divided by sucrose remaining in solution, and usually are
8–18 stationary partitions or compartments, each expressed as the ratio of the polarization value
heated by steam. Continuous vacuum pans are to the total solids as measured by a Brix refrac-
used in both the cane and beet sugar industries. tometer. The differences among the four major
Sugar and Other Sweeteners 947
crystallization boiling schemes are summarized massecuite is fed into the basket through a short
in Table 2. chute from the holding vessel. As the basket
The A and B massecuites, after being rotates, the massecuite forms a vertical layer on
discharged from a vacuum pan, are sent to the screen lining. When the machine reaches
centrifugals for separation. The A and B sugars operating speed (1000–1800 rpm), the syrup
are combined to become commercial raw sugar, flows through the perforations lining the basket
the principal product of a cane sugar factory. The and is removed through an outlet at the bottom of
C massecuite is a low-purity, highly viscous the casing. The sugar on the lining is washed with
material that is not immediately sent to the a spray of water to decrease the amount of molas-
centrifugals because of the large amount of ses adhering to the crystals. The basket continues
recoverable sucrose remaining in solution. to rotate until the sugar is fairly dry, at which
Instead, it is placed in crystallizers, U-shaped time the machine is switched off and brakes
horizontal containers equipped with coils applied. The sugar is discharged by an
attached to a hollow rotating shaft through automatic plow.
which water circulates. The massecuite remains In continuous centrifugals, the machines do
in the crystallizer from 1 to 4 days to allow not stop, but continue in motion while receiving
additional crystallization to take place. Centrifu- fresh supplies of massecuites. The rate of feed
gation of the C massecuite yields a final molasses must be carefully regulated to obtain the opti-
(blackstrap molasses) and a C sugar that is used mum separation of molasses from crystals, while
for seeding the A and B boilings. at the same time not abrading or breaking too
many crystals.
Centrifugation. Massecuite from the vacuum
pans is sent to centrifugal machines in which Raw sugar. The final product of the mill is raw
the crystals are separated from the mother liquor. sugar, about 98.0–99.5% purity, a bulk commod-
A centrifugal consists of a cylindrical, perforated ity shipped around the world to be refined by
basket lined with a screen of perforated sheet importing countries. All raw sugar produced in
metal. The basket, enclosed in a metal casing, is the United States is refined within the United
mounted on a vertical shaft that rotates the bas- States; none is shipped offshore. The quality of
ket, imparting centrifugal force to the raw sugar is determined by its polarization (i.e.,
massecuite. In a batch centrifugal, hot purity), color, moisture, ash, dextran, starch,
948 G. Eggleston et al.
invert (i.e., glucose and fructose content), crystal Molasses exhaustion. Molasses contains a signif-
uniformity, and proportion of color on the crystal icant amount of sucrose and its maximum
surface. These parameters determine the com- exhaustibility (removal of sucrose) has always
mercial price of raw sugar. been a priority for the sugar industry since the
largest loss of sugar occurs in molasses. Well-
Control. Factory control is based on temperature, exhausted cane molasses contains about 33–35%
pH, and purity (polarization). Cane is tested by sucrose. Exhaustion depends on the amount of
various means as it comes to the factory to deter- sucrose in solution, which in turn is largely
mine its characteristics and to determine the affected by the amount of water. Many factors
amount to pay the grower. Control of microbial contribute to poorly exhausted molasses, besides
infection, discussed above, is important. If there inefficiency of process, low water amount, and
is a problem with dextran, dextranase enzyme viscosity, and these include the impurities pres-
can be added to mitigate its negative effects ent in the cane juice. Many of these impurities,
[58]. The optimal application of dextranase is to such as polysaccharides, ash components, and
add concentrated dextranase to juice at ~49 C, organic acids, are melassigenic (i.e., they
where >84% hydrolysis of dextran can be increase the solubility of sucrose and loss of
achieved [58]. Although adding dextranase to sugar in molasses), making sucrose more difficult
syrup can break down some dextran, it is consid- to crystallize and, therefore, going preferentially
erably more expensive than adding to juice. It is into the molasses [62]. The non-sucrose/water
also important that factories measure the activity ratio (qns/w) is useful in gauging molasses
of the dextranase to be added as this can vary exhaustion since it is highly correlated with vis-
widely, and a factory method is available cosity [46]. Target purity is typically the lowest
[58]. The starch content of juice from immature molasses purity achievable in a laboratory or the
sugarcane, as well as certain varieties of sugar- target realistically achievable in a factory. The
cane, can be significant (e.g., in Louisiana and target purity difference (TPD) is the difference
South Africa). α-amylase enzyme can be added between actual molasses purity and the target
to control both insoluble and soluble starch purity, with a low TPD indicating good molasses
forms. If not controlled, starch, especially insol- exhaustion. All target purity equations take
uble starch, can cause severe viscosity problems. reducing sugars and ash effects into account in
If intermediate temperature (IT) stable amylase the ratio of reducing sugars/ash.
(sourced from Bacillus subtilis) is added, then the
best combination is adding it simultaneously to
the clarification tank, next-to-the-last evaporator,
Crystal Quality
and last evaporator [59]. If high temperature
(HT) stable amylase (sourced from Bacillus
Sucrose forms anhydrous monoclinic crystals of
licheniformis) is added, then it may cause
the sphenoidic class [63]. In appearance, the
unwanted carryover (residual) amylase in the
ideal sugar crystal is a slightly asymmetrical
raw sugar. To overcome this, HT amylase should
square with 8–14 faces or planes (Fig. 10).
only be added in the clarification tank and subse-
Certain impurities in the mother liquor can affect
quently treated with powdered activated carbon,
the growth of the sugar crystal and change its
at the factory or refinery, to remove the residual
morphology. Figure 11 shows the elongating
amylase [60]. Recently, a new HT amylase was
effect (along the C-axis) that dextran and
developed for the sugar industry [61] that
associated oligosaccharides have on the crystal
completely denatures in the clarification tank
shape. Sucrose also can form twinned crystals.
after starch is hydrolyzed, and would not require
Figure 12 shows refined sugar crystals.
the PAC treatment.
Sugar and Other Sweeteners 949
Bagasse is the fibrous fraction of the sugarcane technological improvements leading to higher
stalk that remains after juice extraction. When efficiency cogeneration of electricity from
discharged from the milling tandem, bagasse bagasse, in particular the use of new high-
contains approximately 50% by weight of water. pressure boilers, i.e., up to 100 bar (producing
The average fuel value of ash-free dry bagasse is superheated steam at 525 C) [66]. In Brazil,
8300 BTU/lb. (gross calorific value 19,400 kJ/kg during the 2009/2010 harvesting season, the
dry, ash free). It is a valuable by-product because total electricity produced from sugarcane bagasse
it is used to cogenerate steam and electricity for was 20,031 GWh and that value may rise up to
running the factory [64], making cane factories 68,730 GWh in the next 9 years, as long as all
essentially energy-sufficient. Some countries’ factories install 99 bar boilers and 1.04 billion
sugar industries, e.g., Brazil, Mauritius, India, tons of sugarcane is produced [66]. Excess
Australia, Columbia, and Guatemala, operate bagasse can be used to produce paperboard and
large-scale cogeneration of electricity and sell wallboard and as a chemical feedstock for con-
the surplus electricity to the local or national version to furfural, lignocellulosic ethanol and
grid [65]. In recent years, there have been major other biofuels and syngas from Fischer–Tropsch
950 G. Eggleston et al.
(FT) processes [65]. Another option for excess sulfur treatment and filtered. The resulting
bagasse and sugarcane trash (leaves and tops syrup is subjected to a three- or four-boiling
removed in the field or at the factory) is thermo- system with the A and B sugars used as the
chemical conversion to biochars. Biochars can be white sugar product.
applied to soils as a soil amendment and improve
soil fertility. Other applications of biochar are as a
fuel, adsorbent, and for carbon sequestration [65]. Edible Products from the Sugarcane
Factory
water
Mingler
Raw Melter Clarification
and Decolorization
Sugar Affination
washed
filtration
raw
sugar
White, Refined
Sugar
Vacuum
Centrifugation Crystallization
Molasses
raw sugar is mixed with saturated sugar syrup insoluble calcium phosphate precipitates with
(72–75 Brix) at ~50 C in a U-shaped trough many of the impurities in the raw liquor. Simple
called a mingler. Saturated syrup is used to liming is rarely used in refining. The important
avoid dissolving the raw sugar. The mingler has clarification processes are phosphatation and
a rotating agitator to maintain maximum contact carbonatation, which include combinations of
between the sugar and the syrup. The mixture is lime with either phosphoric acid or carbon
centrifuged to separate the crystals from the dioxide.
syrup, and the crystals are then washed with a
small spray of hot water or steam. The “washed” Phosphatation. In phosphatation, the screened
or “affined” sugar is “melted” or dissolved in liquor is heated to 60–70 C and mixed with
water to a density of 55–65 Brix. Potable water, phosphoric acid (0.005–0.025% P2O5 on solids).
steam condensate, and “sweet waters” are used The mixture is immediately limed to pH ~8.0,
for dissolution. The liquor from the melter is aerated with compressed air, and sent to a clari-
screened to remove insoluble matter, such as fier, a tank equipped with heating coils. The
sand, stones, wood, cane fibers, and lint. Screen- liquor enters the clarifier at one end and is heated
ing is done by vibrating screens, cyclonic to ~88 C while flowing to the outlet at the
separators, or centrifugal screens. opposite end. A flocculent precipitate of calcium
Today, most refiners have eliminated the phosphate forms, reacting with or entrapping
affination stage by buying very high purity colloids, organic acids, some coloring matter,
(VHP), very very high purity (VVHP), or very and suspended particles. Air flotation is used to
low color (VLC) raw sugar, in effect, requiring separate the precipitate from the liquor, causing
the raw sugar factory manufacture high purity it to rise to the top of the clarifier as a blanket of
raw sugars. scum, which is skimmed off by moving paddles.
(This process is sometimes known as
phosflotation.) Approximately 25–30% of the
Purification color is removed in this process. In general,
phosphatation is not sensitive to starch, but
The melted liquor is subsequently purified by any recently there have been concerns about insolu-
of several combinations that include clarification ble starch creating unwanted channels in
and decolorization. During clarification, the ion-exchange resins and interfering with other
liquor is treated chemically to remove suspended refinery decolorization processes [Jack
matter, colloids, and other turbid particles. Thompson, LSR Refinery, personal
Clarified liquor is optically clear, but still highly communication].
colored, thus it has to be subsequently
decolorized. Decolorization procedures include Talofloc process (color precipitation). The addi-
treating the clarified liquor with various filtration tion of flocculants and surfactants has greatly
media, such as bone char, granular activated car- improved the simple phosphatation process. The
bon (GAC), powdered activated carbon (PAC), Talofloc process (developed by Tate & Lyle)
or ion-exchange resin, either alone or in some consists of adding a cationic surfactant (Talofloc)
combination. It is necessary to clarify the liquor to the raw melt liquor in concentrations ranging
before the decolorization process because the from 0.02 to 0.07% on solids. This is followed by
particulate impurities will quickly “blind” or the addition of lime and phosphoric acid and the
foul the filtration material and render it useless. incorporation of air. Just before the liquor enters
the clarifying chamber, a polyacrylamide floccu-
Clarification. All clarification treatments include lant (Taloflote) is added that induces aggregation
the addition of lime. Lime increases the pH, of the calcium phosphate precipitate, causing a
stabilizing the sucrose against acid hydrolysis at faster and more complete separation of the
high temperatures, and the calcium forms impurities. As much as 60% of the color can be
Sugar and Other Sweeteners 953
removed by this process. Other similar additives flow rate drops below a predetermined level,
are commercially available. ending the filtration cycle. The calcium carbon-
ate particles in carbonated liquor act as a fairly
Carbonatation. In carbonatation (sometimes also good filter aid medium, as long as the particles
known as carbonation), the melter liquor is are developed to optimum size during
heated to ~60–80 C, limed to ~pH 10–11 carbonatation. Large quantities of
(0.4–0.8% CaO on solids), gassed with carbon polysaccharides (starch, dextran, and others) in
dioxide, heated to ~85 C, and regassed until the the melt liquor can restrict the growth of calcium
pH drops to ~8.5. Because of the two-stage gas- carbonate, requiring the use of diatomaceous
sing, carbonatation requires two clarifiers, a pri- earth. A filter cycle may last from 2 to 12 h
mary and a secondary. Washed flue gases are the depending upon the quality of the feed liquor.
source of carbon dioxide. The carbonated liquor
resides in tanks called saturators for about 3 h New developments. At least one refinery has, in
to allow growth of the calcium carbonate. recent years, been able to omit all chemical
The calcium carbonate precipitate that forms clarification by using only very high-purity,
entraps some colored matter, colloids, organic low-color raw sugar. Clarification is accom-
acids, and inorganic compounds. The precipitate, plished by a two-stage coarse filtration, followed
known as mud, is removed by filtration, such as by a finer filter-aid filtration. Again, this devel-
Sweetland presses. Carbonatation alone achieves opment is possible only because of the high
about 50% decolorization and, with the quality of the incoming raw sugar.
addition of polycationic additives, can achieve
as much as 70% [76]. Carbonatation, however, Scums and muds. Both phosphatation and
is very sensitive to soluble and insoluble starch carbonatation produce scums or muds that have
contents. a moderate level of entrained sucrose, which
There are continuing discussions about the must be recovered or desweetened. Various
merits of one type of clarification over the schemes exist for removing the sugar, such as
other, i.e., phosphatation vs. carbonatation. In secondary clarification of phosphatation scums
summary, the consensus appears to be that and sluicing of carbonation muds with
carbonatation reliably removes more color and dewatering on rotary vacuum filters.
colloidal material and is more flexible in Desweetening streams are, however, susceptible
handling different types of raw sugar, but is to acid degradation of sucrose [77].
more expensive to operate, generates more
waste, is very sensitive to starch, and may have
slightly higher levels of sucrose loss to molasses Decolorization
than phosphatation. Environmental restrictions
on disposal of phosphate-containing waste are a Filtered clarified liquor is a clear orange/brown
consideration for phosphatation refineries. liquid having solids content between 55 and
65 Brix, pH of 6.7–7.2, and temperature between
Filtration. The liquor from phosphatation and 65 and 85 C. The next stage of refining involves
carbonatation contains small amounts of finely removing this color to produce a clear, nearly
dispersed particulate matter that require filtration colorless solution from which white sugar can
for removal. The filtration process is similar for be crystallized. There are basically two major
both types of clarified liquor. A precoat of filter decolorizing processes at the refinery:
aid (diatomaceous earth or perlite) is first depos- (a) chemical and (b) physical.
ited on the filter surfaces of the press. Additional Chemical decolorization.
filter aid is added to phosphate-clarified liquors Chemical decolorization at the factory mainly
to improve press runs. Liquor at 70–85 C is fed involves the use of oxidative decolorizers, espe-
to the press at a pressure of about 60 psi until the cially sulfur dioxide, ozone, and hydrogen
954 G. Eggleston et al.
Table 3 Overall techno-economic comparison of four physical decolorization processes used in sugarcane refineries
[46, 89]
Parameters Bone Char GAC PAC Ion Exchange
Decolorization Low to Medium High Very High Medium
efficiency Also removes ash Does not remove all
colorants
Capital cost Very High High Low Medium to High
Operational cost Very High High Medium Medium
Operational Low Medium High Medium
flexibility pH drop—have to add
magnesite
Environmental Very High Very High Medium High
impact Kilns use energy and Kilns use energy and Solid waste Have to dispose brine
emit CO2; high sweet emit CO2; high sweet with BODb
water water
Other Affected by gums, etc. Affected by gums, etc. Removes odor, No pH drop. High ash
considerations Ash removed but Not affected by ash. insoluble starch, inhibits decolorization.
inhibits decolorization Difficult to automate and amylase Fouling possible
proteina
a
From [60]
b
BOD biological oxygen demand
peroxide. There has been an increasing trend in bone char only moderately remove colorants,
the sugar industry to use such decolorizers but but a considerable amount of the ash components
with limited benefits. Oxidative decolorizers are removed (Table 3). Some refineries in
have three main effects: (a) direct destruction of Columbia use bone char for ash removal only.
colorants (bleaching effect), particularly low Bone char (granular beads of 1–1.5 mm) is gen-
molecular weight flavonoids and phenolic erally packed into cylindrical columns 6.1–7.6 m
compounds, (b) destruction of color precursors high and about 3.1 m in diameter. Liquor flow
to limit later color formation, and (c) increasing through bone char is about 1500 gal/h over
the ionic character of colorants to improve color 30–60 h. After washing, the spent carbonaceous
removal by ion exchange. As long as the pH is adsorbent is transferred to regenerating equip-
held at neutral or below during oxidation, there ment consisting of dryers, kilns, and coolers.
should be no danger of destroying sugars Bone char is regenerated at 540–600 C in a
[78]. Sulfur dioxide (SO2) is most commonly controlled amount of air. After regeneration, the
used in the factory, but is sometimes used in the adsorbent is returned to the system for a new
refinery in certain countries. Ozone (O3) is a decolorizing cycle. The final consumption of
stronger oxidant than hydrogen peroxide (H2O2) bone char is ~0.1–0.3% on melt [81].
with a greater range of oxidation reactions. Davis Granular Activated Carbon (GAC) by itself
et al. [78] showed that ozone at 250 ppm can only removes color; it is usually treated with mag-
decrease syrup color by 33%. However, ozone is nesium oxide (magnesite) to buffer the sugar liquor
expensive to produce and Moodley et al. [79] and may remove a small amount of ash. Compared
stated it was not cost-effective for syrup to bone char it has a much higher surface area
decolorization. (800–2000 m2/g) and thus removes considerably
Physical decolorization. more color mostly via physical absorption onto it
Bone char consists of sintered long bones of by Van der Waal forces [81]. GAC (beads of
cattle, and is composed of calcium hydroxyapa- 1–2 mm) is packed into either pulsed bet or fixed
tite (80–85%) in a carbon matrix. Due to its bed columns. Liquor flow through GAC columns is
relatively low surface area (~100 m2/g) [80], ~3000 gal/h for 20–30 days. Like bone char, GAC
Sugar and Other Sweeteners 955
has to be reactivated in kilns outside of the column; organic fouling. Styrenic resins, although having
GAC is typically revivified at 950–980 C in a less capacity, can remove the remaining small
limited oxygen and steam atmosphere (Table 2). molecular weight colorants. Because styrenic
The final consumption of GAC is ~0.035–0.05% resins will foul more easily, acrylic resins are
on melt, and less is lost in the kiln compared to bone usually placed ahead of them to protect from
char [81]. fouling, and they are used mainly for “polishing”
Powdered Activated Carbon (PAC) has an the fine liquor to remove the final traces of color.
extremely high surface area (up to 2000 mg2/g) Both types of resins have ion exchange as the
and is becoming more commonly used in primary mechanism for color removal; styrene
refineries. It is utilized by mixing it with clear resins also exhibit an adsorption mechanism for
liquor in a tank for up to 20 min. PAC is added at color removal [82]. In recent years, ion-exchange
a dose of 400–1800 ppm often with body feed systems have made use of fractal technology to
(filter aid) of the same concentration [81]. The improve flow and prevent excess pressure drop.
hot, mixed slurry is then filtered through a pres- Compared to activated carbon, IEX resins are not
sure filter or a plant and frame filter press; the as good at removing phenolic/flavonoid
PAC and filter aid are removed from the filter colorants [83].
after completing the duty cycle (typically An overall comparison of four physical decol-
5–10 h). The filter is desweetened by back- orization procesess is listed in Table 3.
flushing with hot water and, depending on the
type of filter employed, the cake can be disposed
of wet or dry [81]. PAC is highly efficient in Crystallization
removing colorants (Table 3), particularly phe-
nolic and flavonoids, but has also been shown to Decolorized liquor is a pale yellow liquid (Inter-
remove insoluble starch and residual amylase national Commission for Uniform Methods of
protein [60] as well as odors. Sugar Analysis [ICUMSA] color 200–300) with
Ion-Exchange Resins (IEX) absorb color and solids content of 55–65% (see section “Process
change the composition of the ash. Since most Control and Instrumentation” for further infor-
sugar colorants are anionic, strong base anionic mation on ICUMSA). This liquor goes to
resins are utilized. Adsorption of sugar colorants multiple-effect evaporators to be concentrated
by IEX is governed by colorant molecular weight to a solids content of ~72 Brix, and then pumped
and charge density, type of charge, pH and ionic to the “white pans” for crystallization. There are
strength of the medium [81]. Typically, IEX four stages in the crystallization process:
resins are utilized in a vessel, with another vessel (a) seeding or graining; (b) establishing the
for regeneration. Ion-exchange resins are packed seed; (c) growth of crystals; and
into vessels 2.4–3.1 m high and 1.8–3.1 m in (d) concentration. Crystallization is governed
diameter, holding between 2.8 and 8.5 m3 of by the degree of supersaturation, which is the
resin. Flow rates of hot (~85 C), filtered melt state in which more solids are in a solution than
are rapid (3000–4500 gal/h), and the cycle is can be dissolved by water at a given temperature.
short (8–20 h). Regeneration is accomplished in (The supersaturation coefficient is defined as the
a vessel with a 10–15% salt solution at 45–60 C; mass fraction of sucrose in water divided by the
before regeneration occurs, the IEX is mass fraction of sucrose in water in a saturated
desweetened by back-flushing with hot water to solution at a given temperature.) There are three
remove any suspended matter. The chloride form phases of supersaturation: [84]
of a strong anionic resin decolorizes the liquor.
IEX resins can be either acrylic or styrenic in 1. The metastable phase—existing crystals grow
composition. Acrylic resins have a higher capac- in size, but no new ones form.
ity for color removal, especially for high molec- 2. The intermediate phase—existing crystals
ular weight color bodies, and good resistance to continue to grow and new ones form.
956 G. Eggleston et al.
3. The labile phase—crystals form spontane- syrup for remelt, or as syrup for producing brown
ously without the presence of others. sugar, also called “soft” sugar in the industry.
Sugar boiling for crystallization is undertaken Centrifuging. Refined sugar crystals are recov-
in the metastable and intermediate phase; below ered from the mother liquor by centrifuging the
the metastable zone, crystals dissolve and massecuite in equipment similar to that used for
inefficiencies result; above the intermediate affining raw sugar. However, at this point, the
phase, uncontrolled “false grain” or extra, small, crystals are washed with a greater quantity of hot
and agglomerated crystals form, resulting in water. The washed crystals are discharged into a
poor-quality crystals. When the syrup is in the holding bin supplying a dryer.
metastable phase, it is “seeded”; that is, a
predetermined amount of very small crystals is Drying and conditioning. Sugar from the
added, which act as nuclei for crystal growth. A centrifugals contains 1–2% moisture and is too
sufficient quantity of evaporated liquor is drawn wet to be placed in storage or packaged. The wet
into the pan to cover the heating elements, and sugar is fed to drying equipment called
water is evaporated from the syrup until its super- granulators, which are large rotating drums,
saturation coefficient approaches 1.25. At this 4.6–10.7 m long and 1.8–2.1 m in diameter,
point, the steam pressure is lowered, and seed inclined slightly for gravity discharge. Screw
crystals are added. The seed consists of finely conveyors, scrolls, vibratory “grasshoppers,” or
pulverized sugar dispersed in isopropyl alcohol linear belts are used to transport wet sugar from
or sugar liquor. This method is called shock the centrifuge to the drier, where heated air is
seeding because addition of the seed induces an blown through the dryer, concurrent with the
immediate formation of crystal nuclei throughout flow of the sugar. Sugar exiting the granulators
the supersaturated syrup. The nuclei are grown to has a moisture content of about 0.03%.
a predetermined size or grain. Once the grain is
established, the crystals are grown to size by
maintaining supersaturation between 1.25 and Remelt Sugar
1.40 through control of the steam pressure, vac-
uum, and the feed rate of the evaporated liquor. The sugar contained in affination syrup must be
Adequate circulation during crystal growth is recovered for economy, which is accomplished
important. by crystallizing the sugar in a vacuum pan. The
When the volume of the massecuite reaches area of the refinery where various “low-grade
the maximum working capacity of the pan, the boilings” take place is called the remelt house.
syrup feed is shut off, and evaporation is allowed The resulting sugar is “raw” in composition and
to proceed until a thick massecuite is formed. is returned to the refinery at the affination station,
When the massecuite concentration is considered hence it is “remelted.” The residual syrup from
“tight,” the steam and the vacuum are shut off, the remelt station is known as refiners’
and the massecuite is dropped into a holding tank blackstrap, from which no further sugar can be
equipped with agitators, where it is kept in recovered. Various grades or streams of remelt
motion until discharged into the centrifuges. are produced, depending on the refinery.
The boiling system in a refinery is straightfor-
ward. The first strike is boiled from evaporator
liquor; the second strike is boiled from the runoff
syrup of the first strike, continuing on to three or Packaging and Storing Refined
four strikes. These strikes are blended to form the Granulated Sugar
final white sugar product. The runoff of the last
strike, which is quite high in color and ash, can be Sugar leaves the dryer at around 52–55 C and is
used in a variety of ways: as syrup for affination, as allowed to cool to about 45 C. Sugar leaving the
Sugar and Other Sweeteners 957
dryer still contains enough moisture to cause Liquid sugars. Liquid sugars (sugar dissolved in
problems with caking on storage, and the proper water) are economically important because food
bulk storage and conditioning of sugars in silos is manufacturers often prefer to use sugar in the
a widely discussed topic [85, 86]. One of the form of syrup because of the ease of handling a
most important considerations for refined sugar liquid product. Liquid sugars are prepared by one
is its ability to store well, without caking or of two methods: dissolving refined sugar in water;
darkening in color. or further purification of in-process liquors by
Granulated sugar remains free flowing for a ion-exchange treatment to remove minerals, and
longer period of time if it is “conditioned,” as further decolorization using bone char and
conditioning further reduces the moisture level, pulverized or granular carbon. Liquid sugar may
which is necessary to prevent caking. Condition- consist of (a) only sucrose, (b) as a mixture of
ing takes place in large vertical silos, with up to sucrose and invert sugar, or (c) as a blend with
three million pounds capacity. Conditioned various glucose syrups from starch hydrolysis.
dehumidified air is percolated into the sugar Sucrose liquid sugars are usually distributed at a
from the bottom of each silo. Residence times 67% sugar concentration, whereas invert sugar
in silos vary, from about 24 to 72 h. Proper and mixtures of invert and sucrose are distributed
control of air flow, humidity of the air, and tem- at concentrations of 72–77% sugar. Partially
perature are essential for good conditioning. inverted sugar syrups are commercially prefera-
Sugar leaves the silos with a moisture content ble because of the higher solids content and
of 0.025% or less. Following conditioning, the greater microbiological stability.
sugar is screened to meet the particle size Partially inverted sugar syrups are made by
requirements of customers. Screened sugar is one of three hydrolytic methods: acid hydrolysis
then sent for packaging or for transport in bulk. with mineral acids (sulfuric or hydrochloric),
Sugar that is not immediately used is placed in hydrolysis by cation ion-exchange resin, or
storage silos for periods that can be as long as inversion by enzymes. Acid hydrolysis by min-
2 months. Sugar storage is another area where eral acids has the disadvantage that the resulting
problems with caking and solidification can syrups have a high ash content because the solu-
occur due to moisture migration, and newer tion is neutralized with sodium or potassium
systems are beginning to appear where sugar in hydroxide. Enzymatic conversion has the disad-
storage is treated with a slow stream of vantage of being expensive and not very efficient
conditioned air. at the high temperature and densities of the
Granulated sugar is packaged in 1, 5, 10, 25, solutions being hydrolyzed. Cationic resin treat-
50, and 100 lb. bags, 2000 lb. sacks, as well as ment offers the best alternative, resulting in
cartons and heat seal packets. Other packaging nearly ash-free invert syrup. The most popular
configurations are possible. invert syrup is a 50% mixture of sucrose and
invert [88].
Liquid brown syrups are also available,
Specialty Sugars known as refiners syrups, and can be adjusted in
color, flavor, ash level, and sucrose content
The refined sugar is passed through sieves with a according to the specifications of the customer.
specific holes size that determines the largest
grain in any given batch. Some sugars are also Brown or soft sugars. Brown sugars range in
sieved to remove smaller crystals [11]. Refineries color from light to dark brown. They have very
produce a number of specialty sugars and syrups small crystals and high moisture content, ranging
designed to meet the needs of customers. These from 0.5 to 3%. The combination of very small
include sugars with various crystal sizes, pow- crystals and high moisture gives the sugars the
dered sugars, brown sugars, and liquid “soft” appearance and texture. Brown/soft sugars
sugars [87]. also contain higher ash, invert sugar, and an array
958 G. Eggleston et al.
controlled at not much above freezing to mini- namely the movement of juice countercurrent to
mize degradation of the sucrose content. the movement of the cossettes.
The RT-type diffuser is a large revolving
Washing. Beets are transferred from storage to drum with an internal helix that separates the
the factory in water flumes. These flumes lead drum into moving compartments. As the drum
directly into a rock catcher, which allows rocks revolves, the cossettes travel by the action of the
to settle out, and then on into a trash catcher and a moving helix from one end of the drum to the
rotary washer. A large amount of soil usually is other end, while the juice moves in the opposite
entrained with the beet roots, and processes for direction. The BMA diffuser is a cylindrical
recovering and returning the soil to the field are tower with a conveyor mechanism attached to a
in use. central rotating shaft. Guide plates on the shaft
direct the cossettes upward, while the juice exits
Slicing. The washed beets are sliced into thin through screens at the bottom.
V-shaped cossettes by means of specially shaped
knives set in frames mounted around the periph- Beet pulp. Beet pulp is the solid residual portion
ery of a rotating drum. Good removal of rocks remaining after diffusion, and is a valuable
and trash is essential for a reasonable life for the by-product. Wet pulp, containing 85–90% mois-
knives. ture, is dewatered in horizontal double-screw
presses, reducing the moisture content to about
75%. Pulp is further dried to about 8–10% mois-
Extraction of the Juice ture in pulp dryers, direct-fired horizontal rotat-
ing drums. Newer pulp-drying technology,
Diffusion. The process of extracting the juice utilizing a pressurized fluid bed, results in 40%
from the beet is diffusion. The cossettes are more capacity and better energy efficiency
weighed and transferred continuously into a dif- [92]. Beet pulp is mainly used as a pelletized
fuser where water passes countercurrent to the animal feed, either alone or mixed with molasses.
movement of the cossettes and where, by diffu- In the 1980s, several beet companies devel-
sion, sugar and some of the nonsugars of the beet oped edible fiber from beet pulp to take advantage
are extracted. For optimum extraction of juice, of interest in the health benefits of dietary fiber
the sucrose-containing plant cells need to be fully [93]. The fiber has a high water-holding capacity
disrupted to allow the escape of the juice. This is and other interesting properties, but the market
done mechanically (5–15% of cells are disrupted has remained small and specialized, with uses as a
by the slicers) and with heat. A balance between fiber additive in both human and pet food.
temperature and the time of heating is necessary:
it should be high enough to maximally extract the
juice, but not so high as to cause extraction of Juice Purification
undesirable nonsugars, such as pectins, or to
cause color formation and sugar degradation. The diffusion juice (also called raw juice) is a
The temperature of the juices during diffusion turbid liquid ranging in color from lavender to
is around 70 C. Retention time is ~1 h. Antifoam nearly black, containing 15–18% sucrose and
agents are used to control foam in continuous 1–3% nonsugars, including proteins, nitrogenous
diffusers, and bactericides are added for bases, amino acids, amides, inorganic material,
microbiological control. Continuous diffusers and pectinaceous matter. It also contains 0.25%
have largely replaced batch diffusers. Continu- sodium and potassium. These impurities are
ous diffusers come in a variety of forms and removed by a series of purification processes
shapes, but all employ the same principle, using lime and carbon dioxide (carbonation),
Sugar and Other Sweeteners 961
and sulfur dioxide (sulfitation). In recent years, gassing with carbon dioxide. The carbon dioxide
there has been some use of ion-exchange resins reacts with the lime to form calcium carbonate,
to produce high-quality refined granulated sugar. which helps to absorb the insoluble impurities,
Knowledge of the chemistry of the raw beet and some of the soluble impurities as well. The
juice is important in controlling the phases of resulting mixture, containing insoluble lime
juice purification. The addition of increasing salts, is pumped to subsiders (thickeners,
amounts of lime and carbon dioxide should pre- clarifiers) to remove the insolubles by settling
cipitate pectinaceous materials and insoluble (sludge separation), and clarified juice is
anions such as phosphate, sulfate, oxalate, and decanted. From the subsider, the partially
others, as calcium salts cause alkaline degrada- clarified filtrate is recarbonated (second carbon-
tion of invert sugar into lactic and other acids, ation) to lower the pH further, and the residual
and flocculation of colorants. Lime is also essen- lime is precipitated. The juice is then treated with
tial for promoting good filtration. about 150 ppm sulfur dioxide gas (sulfitation),
Classic juice purification consists of which helps to inhibit further color-forming
preliming, main liming, first carbonation, first reactions in the juice, removes any remaining
sludge separation (clarification), second carbon- traces of calcium, and provides the final pH
ation, second sludge separation, sulfitation, and adjustment, to a pH of around 8–8.5. This treat-
filtration. Control of pH is very important ment is followed by press filtration. The sludge
throughout the process and depends on the qual- from the subsiders is filtered on rotary-drum
ity of the beet juice, which is determined in the filters, and the sugar-containing filtrate is
lab. returned to the first carbonation step. The carbon-
ation process can be either continuous or batch.
Preliming. A small amount of lime (0.12–0.3%) In some factories, the clarified juice is also sent
CaO is added to the juice, increasing the juice pH to softeners (cation resins) to remove any
from about 6.2 to 10.8–11.4. The lime reacts with remaining calcium.
nonsugar impurities in the juice to make insolu- Beet processing uses a large amount of lime
ble precipitates and soluble products. Calcium (2–2.5% on beet) and efforts are being made to
carbonate in the form of recycled first carbon- reduce the usage by effective control of tempera-
ation sludge is added to provide colloid adsorp- ture, pH, and other parameters [94], which can
tion and stabilization. Temperature may be cool bring down usage to about 1.0–1.2% and inclu-
(50 C) or hot (80 C) depending on the factory sion of innovative processes, such as membrane
design. Insoluble precipitates are formed filtration [95], which can further reduce lime
quickly. Retention time is 15–30 min. usage to around 0.8% on beets. Beet juice
clarification is also considerably more suscepti-
Main liming. The addition of more lime (main ble to lower concentrations of dextran than
liming) to an alkalinity of 0.8–1.5% CaO on juice sugarcane juice clarification [96]. Dextranase
results in a second set of reactions that produce application to the beet juice, however, has been
soluble products. During these reactions, the optimized to improve clarification [96]. The
small amount of invert sugar present in the raw recovery of lime by reburning is also being stud-
juice is destroyed and amides are saponified. ied. The clarified juice is called “thin juice” and
These reactions help to stabilize the juice and contains about 15% solids.
reduce color formation. A great deal of color is
formed during this stage, but this type of
alkaline-derived colorant is fairly easy to remove Evaporation and Standard Liquor
in crystallization.
The thin juice discharged from the filter presses
First and second carbonation. In this process, after clarification is evaporated to “thick juice”
heated, limed juice is sent to a carbonator for or evaporator syrup (50–65% solids) in multiple-
962 G. Eggleston et al.
effect evaporators, containing five, six, or even A major difference between cane and beet
seven effects. If decolorizing absorbents are sugar refining is that beet refining occurs in one
used, they are usually added to the thick juice. stage, with refined sugar produced directly from
Granular and powdered activated carbons have the sugar beets, whereas refined cane sugar is
been used for this purpose. Thick juice that has produced first as a raw sugar and then refined. It
been treated with powdered activated carbon is possible for beet sugar to be produced directly
usually must be double filtered to remove all because the nature of the coloring material in
the carbon. beet sugar is fundamentally different from that
Low raw sugars (sugars with purities below of cane. A beet evaporator syrup with color >
that of refined sugar) and white centrifugal wash 3000 ICUMSA color units produces a white
water are added to the thick juice in the melters to sugar with an ICUMSA color of 25–40. How-
make “standard liquor” from which white sugar ever, for a cane white sugar of the same color to
is crystallized. Standard liquor is usually filtered be produced, the color of the evaporator syrup
with diatomaceous earth before going to the vac- must be only 200–300 color units. The nature of
uum pan. these differences appears to be associated with
lower molecular weight colorants in beet, lower
polysaccharide content in beet, and colorant
mainly composed of alkaline degradation
Extending the Processing Cycle products of invert sugar [98].
literature [100, 101]. Up to 90% of the sucrose in concentration which has to be “softened” before
the molasses can be recovered and other valuable it can be put on a resin. Therefore, cane molasses
products, such as betaine, can also be recovered. must be clarified to remove suspended matter and
Most beet factories today desugarize molasses. gums, and prior softening is necessary to extend
Desugarization is accomplished using cross- the life of the resin. The resulting product frac-
linked strong cationic resin in the potassium tion from cane molasses contains a mixture of
form. Sucrose is preferentially absorbed by the sucrose and reducing sugars. There has been little
ion-exchange resin and separates by lagging adoption of this process in the cane sugar
behind the majority of the nonsucrose industry [103].
components. Continuous processes are based on
countercurrent technology. The SMB process
avoids mechanical movement of resin, keeping Process Control and Instrumentation
the whole resin bed stationary while changing
product inlets and outlets with an internal circu- The sugar industry has always been in the fore-
lar flow. Typically, molasses SMB systems have front of chemical control. The most important
8–20 resin compartments (or cells) in series. The areas of control include measurement of sugar
countercurrent resin movement is simulated by (sucrose) content (done by polarization), pH con-
changing the inlet and outlet ports forward in the trol (because sugar is unstable at low pH, and
direction of the liquid flow. In coupled loop more so when high temperatures prevail), color
technology, developed by Amalgamated Sugar measurement, and control of vacuum pans (for
in the 1990s, a cascade of several loops is efficient crystallization).
provided instead of connecting several individual At the end of the nineteenth century,
cells. This allows recovery of additional ICUMSA (International Commission for
nonsucrose components, such as betaine, and Uniform Methods in Sugar Analysis) was
provides a purer sucrose fraction. For proper formed. This organization, which continues
operation of a molasses desugarization plant, today, is dedicated to all aspects of sugar analy-
the molasses must be low in calcium and magne- sis, validation of methods, and promulgating offi-
sium ions (this is usually achieved by thin juice cial methods that are scientifically valid and can
softening), free of suspended solids, and free of be used for trade. A good early history of
oxygen, which irreversibly damages the resin ICUMSA, covering the first session in 1897 up
[102]. The sucrose fraction, called “extract,” to 1936, can be found in Bates [104].
goes to pan crystallization, is mixed with thick Raw sugar quality characteristics that are
juice, and crystallized, or is further purified with measured include polarization, color, grain size,
activated carbon or ion-exchange resin and sold moisture, invert, dextran, starch, and surface
as liquid sugar. The waste fraction, called the color (color that could be removed in affination).
“raffinate,” is concentrated and sold as fodder New techniques, such as gas chromatography,
molasses. enzymes, high-pressure liquid chromatography
(HPLC), and near infrared (NIR) analysis, are
in use for determining various parameters, par-
Desugarization of Cane Molasses ticularly sucrose, glucose, and fructose. NIR is
particularly promising because it is nondestruc-
Desugarization of cane molasses is more difficult tive and can theoretically measure a wide range
and less economical for several reasons: it has a of parameters, such as moisture in bagasse and
lower content of sucrose (about 35%) and a polarization of juice. These methods are coming
higher content of invert sugar (about 10%); it is to the forefront because the older method of
more viscous because of higher concentrations of determining sugar content, polarization, has sev-
polysaccharides; it has a lot more suspended eral drawbacks. Originally, lead acetate was used
material, and it has a higher salt and calcium to clarify solutions for polarization
964 G. Eggleston et al.
Table 4 Major sugar-producing countries, 2015/2016 (world centrifugal sugar production in units of one million
metric tons) [1, 107]
Total sugar production Million Metric Tons, Raw Value Source
Brazil 39 Cane
India 26 Cane
European Union 16 Mostly beet
Thailand 10.4 Cane
China 10 90% from cane, 10% beet
United States 9 56.8% beet; 43.2% cane
Mexico 6.4 Cane
Pakistan 5.4 Mostly cane
Australia 5 Cane
Russia 4.7 Beet
Table 5 Per capita consumption of different world regions since 2011/2012 [1]
World Sugar Consumption in million metric tons, raw value
World Region 2011/2012 2012/2013 2013/2014 2014/2015 2015/2016
European Union 19.02 19.09 19.22 19.45 19.33
Europea 31.05 31.14 31.28 31.39 31.20
Africa 18.47 19.17 19.63 20.28 20.91
North and Central America 19.59 20.45 20.76 20.89 21.08
South America 21.06 21.06 21.09 21.29 21.23
Asia 76.55 78.88 81.35 83.56 85.53
Oceania 1.70 1.70 1.71 1.71 1.71
Total: 168.42 172.39 175.81 179.12 181.66
a
Includes the European Union plus other countries in the European continent including Turkey
measurement; with lead use restricted in most inversely proportional to the viscosity of the
countries, aluminum and zinc salts have replaced solution, which in turn has a similar relation-
it, but these are not as effective as clarifiers. ship to the water content and thus the degree
Polarization is also not a direct measurement of of supersaturation.
sucrose, so it can be inaccurate in low-purity 3. Fluidity of the massecuite: An ammeter is
materials, such as molasses. used to measure the current used by the
Instrumentation is used extensively in sugar motor of a mechanical circulator; changes in
boiling to control the process of crystallization. current indicate changes in the fluidity of the
Some of the principles used to provide control of massecuite.
vacuum pans for boiling a strike of sugar are 4. Soluble solids measured by a refractometer.
listed below [84]. 5. Radiofrequency.
6. Microwave density probe [105].
1. Boiling point rise (BPR): thermometers are
used to measure the temperature of the
massecuite and its vapors (the difference
between these two temperatures is the Cane and Beet Sugar Production
observed BPR).
2. Electrical conductivity of the massecuite, Sugar (cane and beet) is produced in approxi-
based on the principle that conductivity is mately 120 countries. Cane sugar is produced in
Sugar and Other Sweeteners 965
Table 6 US sugar deliveries to industrial and nonindustrial users, selected years (1000 short tons, raw value) [108]
Use 1990 1993 1995 2000 2005 2009
Bakery and cereal products 1608 1785 1905 2264 2297 2286
Confectionery products 1279 1292 1372 1328 1131 1082
Ice cream and dairy products 462 424 452 499 587 577
Beverages 228 158 169 168 237 351
Canned, bottled, and frozen foods 332 336 279 330 336 427
All other food uses 642 725 864 817 606 572
Nonfood use 102 85 64 85 92 83
Total industrial use 4660 4805 5103 5491 5286 5377
Hotels, restaurants, and institutions 108 108 103 71 115 127
Wholesale grocers, jobbers, sugar dealers 2130 2075 2173 2241 2401 2352
Retail grocers, chain stores 1077 1235 1236 1242 1262 1241
All other deliveries 76 171 189 339 248 179
Total nonindustrial use 3391 3589 3701 3893 4020 3899
Total United States 8051 8394 8804 9383 9312 9276
tropical and subtropical areas, and beet sugar is links with obesity and medical diseases such as
produced in temperate zones. The United States diabetes [6].
is sixth among the world’s sugar-producing How sugars are utilized for industrial and
areas, and is the only country with significant nonindustrial uses is summarized in Table 6.
sugarcane and sugar beet acreage. Cane sugar Nonfood uses of sucrose constitute only a small
production is approximately 80.4% of the world portion of total use [108].
sugar production and beet sugar is 19.6%. The
major producers of sugarcane and beet sugar are
shown in Table 4. The biggest change to occur in
Derivatives of Sucrose:
world sugar production is the ascension of Brazil
Sucrochemistry
as the major producer and exporter [106]. Brazil,
India, and the European Union alone account for
Because of its high purity and wide availability,
46% of world sugar production.
sucrose has been viewed as an attractive feedstock
for organic chemical synthesis. Sucrochemistry
has been pursued for many years, and many
Sugar Consumption and Usage products have been produced [109–111]. How-
ever, the economics of production have not been
Per capita consumption of sugar varies widely good and the reactivity of sucrose is difficult to
from country to country, and is often a measure control. Among the derivatives of sucrose are
of the affluence and level of industrial develop- ethers, fatty and other esters, acetals, and reduc-
ment of a country, except in Asia, where dietary tion products. Successful products from sucrose
customs do not typically include high include surfactants, surface coatings, food and
sugar intake. However, as shown in Table 5, feed additives, polymers, textile chemicals,
consumption has been increasing in Asia, Africa, pharmaceuticals, and pesticides. A promising
and North and Central America. The increase in development is the conversion of sugar-based
the Americas is at least partially because of feedstocks into conventional liquid fuels and
the current backlash against high fructose corn chemicals using a patented catalytic aqueous
syrup (HFCS). The demand for high fructose phase reforming process [112]. Other sucrose-
corn syrup (HFCS) has decreased in recent based products in successful commercial distribu-
years due to multiple consumer issues, tion include olestra, a liquid sucrose polyester fat
including high fructose content, GMO, and substitute, sucrose acetate isobutyrate, and
966 G. Eggleston et al.
gelatinization, liquefaction, and saccharification. products, as shown in Table 7. HFCSs are classi-
Liquefaction refers to the acid- or enzyme- fied according to the fructose content, as a per-
catalyzed conversion of starch into maltodextrin. cent of solids (i.e., 42%, 55%, 90%), rather than
Starch, usually from wet milling of corn, is by DE. Table 8 shows the composition of various
pumped as a slurry to the conversion plant, corn syrups. In addition to carbohydrates, the
where it undergoes one or more hydrolytic pro- syrups contain some sodium chloride and traces
cesses to yield mixtures of various carbohydrates of nitrogenous substances. Maltodextrin is a
in the form of syrups. The type and amount of the dried corn syrup having a DE below 20, whereas
various carbohydrates obtained depend upon the the dry dextrins with a DE above 20 are called
type of hydrolysis system used (acid, acid– corn syrup solids.
enzyme, or enzyme–enzyme), the extent to
which the hydrolytic reaction is allowed to pro-
ceed, and the type of enzyme(s) used. The fact Acid Hydrolysis of Starch
that most starches consist of two different kinds
of polymers (amylose and amylopectin) also As mentioned above, this process now serves
influences the nature of the products obtained. mainly as an adjunct to enzymatic conversion
The extent to which starch is converted into of starch and is rarely used alone. A starch slurry
simpler carbohydrates is indicated by the dex- containing 35–45% solids is acidified with
trose equivalent (DE), a measure of the reducing hydrochloric acid to about pH 1.8–1.9. The sus-
sugar content calculated as dextrose and pension is pumped into an autoclave (converter)
expressed as a percentage of the dry substances. where live steam is gradually admitted to a pres-
Hydrolyzates having dextrose equivalents rang- sure of 30–45 psi. The conversion time largely
ing from 5 to 100 are produced. Those having a determines the DE of the hydrolyzate; for exam-
low dextrose equivalent frequently are referred to ple, 8 min may produce 42 DE syrup, and 10 min
as dextrins and are not sweet. They are produced may produce 55 DE [118]. Converted liquors are
by minimal acid hydrolysis or roasting. Starch neutralized with sodium carbonate to a pH of
hydrolyzate syrups commonly are produced as 5–7, with coagulation of insoluble protein, fats,
“low,” “intermediate,” “high,” or “very-high” and colloidal matter. The scum is removed by
conversion products, as more or less standard centrifugation.
The dark-colored clarified liquor is pressure-
filtered and concentrated to 60% solids in
Table 7 Conversion groups for starch hydrolyzates multiple-effect evaporators. The concentrated
Conversion DE liquor is decolorized with granular carbon in
Low (Type I) 20–38 columns 3.7 m in diameter and 9.1 m high in a
Intermediate (Type II) 38–58 countercurrent manner; that is, liquor flows
High (Type III) 58–73 upward in the columns, while a portion of the
Very high (Type IV) 73 and above
carbon is removed from the bottom periodically.
Carbon is used at a rate of 2.5% of dry solid
Table 8 Carbohydrate composition of glucose syrups (saccharides as a percent of total carbohydrates) [117]
DE Glucose Maltose Tri-a Tetra-a Penta-a Hexa-a Hepta-a Higher
15 3.7 4.4 4.4 4.5 4.3 3.3 3.0 72.4
35 13.4 11.3 10.0 9.1 7.8 6.5 5.5 36.4
45 21.0 14.9 12.2 10.1 8.4 6.5 5.6 21.3
55 30.8 18.1 13.2 9.5 7.2 5.1 4.2 11.9
65 42.5 20.9 12.7 7.5 5.1 3.6 2.2 5.5
a
Refers to the number of glucose units in the oligosaccharide: tri maltotriose; tetra maltotetraose; penta maltopentaose,
etc.
968 G. Eggleston et al.
High Fructose Corn Syrup 4–5, and it is purified by ion-exchange resin and
activated carbon. This results in a 42% HFCS.
HFCS is produced from very pure glucose syrup For use in soft drinks, it is converted to 55%
using glucose isomerase. Commercial glucose HFCS by passing through large chromatographic
isomerase is produced from a variety of columns of zeolites or the calcium salts of cation-
microorganisms: Bacillus coagulans, Actino- exchange resins, which absorb and separate the
planes missouriensis, and several Streptomyces fructose from the other components. This
species. Glucose isomerase is always used in produces a stream of about 90% fructose, which
immobilized form because it is an intracellular is then blended with 42% fructose syrup to pro-
enzyme. The isomerization reaction is carried out duce the desired 55% fructose syrup product.
at 60 C at pH 7–8. Reaction time is limited to HFCS technology and products have spread to
prevent degradation of the fructose, which is many countries including Canada, Japan, and
more labile than glucose. All isomerization several western European nations.
reactions today are undertaken in continuous
mode, rather than batch mode. The operating
lifetime of a column of immobilized enzyme Molasses
can be as long as 200–360 days, depending on
the robustness of the enzyme used [120]. Molasses, defined as the residual mother liquor
The basic feature of the isomerization process from which little or no additional sugar can be
is a series of reactors containing the immobilized recovered economically, is a by-product of the
enzyme fixed in a packed bed. The feed material sugarcane, beet, and dextrose industries. Each
is of the highest practical purity possible because type of manufacturer has designated this liquid
enzymatic activity is closely related to the purity by-product with its own name. The molasses
of the glucose syrup. Glucose syrup of about from both raw sugar manufacture and cane
94 DE is filtered, treated with activated carbon sugar refining is commonly named blackstrap
to remove residual color, and deionized with molasses. In the cane factory, it is also known
ion-exchange resin to lower the ash content, par- as final molasses, and in the refinery it is some-
ticularly the calcium ion, which interferes with times named refinery molasses. Molasses
the magnesium enzyme activator. The dissolved from beets is simply named beet molasses.
oxygen is reduced by flash evaporation, which The composition of molasses varies depending
also concentrates the feedstock to 40–45% on location, varieties harvested, and the type and
glucose and raises the temperature to 60–65 C. efficiency of the process operation. The amount
At this point, prior to entering the reactors, mag- of refinery molasses is usually small, because as
nesium ions are added as enzyme activators. The much as possible is recycled, and a lot is utilized
pH is adjusted to ~8. Isomerized liquor is in the manufacture of brown sugar. Some cane
removed from the process when the equivalent refineries have no molasses output at all. The
of 42% fructose on a dryo basis is reached. After general composition of each type of molasses is
isomerization, the pH of the syrup is lowered to shown in Table 9.
970 G. Eggleston et al.
Blackstrap molasses from the sugarcane fac- Table 10 Relative sweetness (RS) of carbohydrate-
tory contains significant quantities of sucrose and based sweeteners
reducing sugars (glucose and fructose); reducing Sweetener RS
sugars are from the cane itself and some are Crystalline fructose 180
formed during the processing of the cane juice Fructose in solution (5–15%) 115–125
by enzymatic and acid hydrolysis of sucrose. High fructose corn syrup 100–130
Refinery blackstrap molasses has fewer Invert syrup 105
Sucrose 100
impurities because the raw sugar starting mate-
Tagatose 92
rial has fewer impurities and more sucrose than
Xylitol (10% solution) 85
the sugarcane juice. Beet molasses contains pri- Xylitol (10% solution) 100
marily sucrose and little or no reducing sugar Xylitol (10% in solution) 120
because of the lower content of reducing sugars Glucose (2% solution) 50
in beet juice and because the highly alkaline Glucose (8–10% solution) 60–70
processing conditions destroy most of the reduc- Glucose (50% solution) 90–100
ing sugars. Furthermore, the sucrose in beet Erythritol 70
molasses is recovered by chromatographic pro- Sorbitol (hydrogenated glucose) 70
cesses described earlier. Maltitol (hydrogenated maltose) 68
The main uses of molasses are for cattle feed, Maltose 50
production of some fermentation products, such Trehalose 45–50
Mannitol 40
as yeast, citric acid, potable and fuel ethanol.
Lactitol (hydrogenated lactose) 30–40
Brazil has been at the forefront of producing fuel
Lactose (milk sugar) 15–30
ethanol from sugarcane, specifically from the
juice and/or molasses. Brazil unveiled the world’s
first alcohol-powered car after the 1970s oil crisis, labeling purposes, so foods containing them as
using its abundant supplies of sugarcane. In spite sweeteners can be called “sugar free.” The
of some difficulties in the 1990s, this innovative polyols are usually 15–30% sweeter than their
program has been considered successful. corresponding sugar (see Table 7). Some of the
polyols give a cooling sensation on the tongue.
Several of the new carbohydrate sweeteners are
Other Sweeteners described below.
Erythritol, 70% as sweet as sucrose, is a
Several carbohydrate-based sweeteners exist on polyol currently used as a bulk sweetener in
the market today. Although sucrose is the “gold reduced-calorie foods. It has only 0.2 cal/g
standard” for sweeteners, other sweeteners have (sucrose has 4 cal/g) and was Generally
gained commercial viability because they are Recognized As Safe (GRAS) by the Food and
less expensive (such as corn-based sweeteners), Drug Administration (FDA) in 1997, allowing it
have fewer calories, or are better suited for dia- to be used in foods in the United States
betic diets. Unlike the synthetic sweeteners, most [123]. Erythritol is produced by fermentation
of the carbohydrate-based sweeteners are less with the fungus Moniliella pollinis [124].
sweet than sucrose, with the notable exception Tagatose, a monosaccharide similar to fruc-
of sucralose, which is 600 times sweeter than tose, received GRAS status from the FDA in
sucrose and is nonnutritive. Fructose and xylitol April 2001. This sugar, 92% as sweet as sucrose,
are reported to be sweeter than sucrose. Table 10 with 1.5 cal/g, is produced from galactose
shows the relative sweetness of the carbohydrate- obtained from whey, using immobilized enzymes
based sweeteners [121, 122]. [125]. It has similar bulking properties to sucrose.
An important group of carbohydrate-based Trehalose, a disaccharide sweetener, 45–50%
sweeteners are the polyols, also known as sugar as sweet as sucrose, was given GRAS status in
alcohols. These are not considered sugars for 2000. It is naturally found in mushrooms, honey,
Sugar and Other Sweeteners 971
lobster, shrimp, and foods made with yeast. It has increased by mogrosides, a group of triterpene
been used in Japan for decades, and is commer- glycosides.
cially produced from starch by bacterial enzymes Other natural sweeteners for other foodstuffs
[126]. Besides its mild sweetening power, it include honey, palm sugars, maple syrup, and
maintains cell structure during freezing and sweet sorghum syrup [11]. Honey was the first
dehydration of foods. It is a nonreducing sugar, sweetener for humans and remained so in the
so it does not participate in the Maillard Western world until the plantation system of
browning reaction and helps to protect the color sugar production was developed. Honey is essen-
of processed foods [127]. tially nectar concentrated by honeybees to ~18%
moisture, and is composed mainly of fructose
and glucose and some novel oligosaccharides.
Honey has been produced and exported for
Other Natural Sweeteners centuries. Today, there is a great emphasis on
the organoleptic qualities of particular honeys
In addition to the aforementioned concerns about produced from specific nectar sources
high fructose corn syrups, there have also been [11]. High-quality honey is regarded as a gour-
consumer concerns about artificial sweeteners met food, whereas a lower-grade honey (baking
such as aspartame and saccharin, causing top honey) is used in the food industry. Palm sugar is
diet soft drinks to be in decline in the USA one of the world’s oldest sweeteners, and is pro-
[128]. Beverage manufacturers have been turn- duced and consumed across large parts of Asia
ing to other natural sweeteners as well as cane [11]. Palm sugar is produced by boiling sap col-
and beet sugars as replacements. These include lected from the cut inflorescence of many palm
agave, stevia, monk fruit, and erythritol varieties, including the date palm. No matter
(described above). Agave syrup (nectar) is a which palm it is made from, palm sugar is less
sweetener extracted from succulent agave plants sweet than cane sugar [11]. Maple syrup is also a
native to the Americas, with most species in sweetener made from intensive evaporation of
Mexico. Agave syrup is high in fructose. Stevia the sap from maple trees (Acer saccharum),
(a glycoside) is a natural sweetener extracted which are grown almost exclusively in the north-
from Stevia rebaudiana (mainly rebaudioside east regions of Canada and the USA. Maple
A), a member of the sunflower family that syrup is primarily sucrose although the darker
originated in Paraguay [11, 128]. Stevia is twenty syrups contain fructose and glucose. It is a fla-
times sweeter than sucrose with no calories. vorful natural product that is in high demand
Purified stevia extracts have GRAS status [11]. Sweet sorghum syrup is a natural sweetener
[128]. Difficulties have been reported with made from the juice of sweet sorghum, a grass
stevia’s bitter aftertaste, especially at the levels cane similar to sugarcane. It was introduced to
needed to produce carbonated soft drinks. There- the USA around 1850 and its potential as a liquid
fore, it has to be formulated with other food sweetener was quickly recognized [11]. By
sweeteners in beverages [128]. Nevertheless, 1890, over 25 million gallons of sweet sorghum
stevia has continued to enjoy a high profile as a syrup was produced across forty-four states in the
sweetener in the past year [114]. Monk fruit USA. It became the predominant table sweetener
sweetener is from a small round fruit (lo han of early America, ultimately being displaced by
guo) grown in Southeast Asia. Monk fruit juice refined white sugar around 1900. Since that time,
concentrate is a natural fruit juice that is 15–20 sweet sorghum has been grown as a boutique
times sweeter than sucrose with low calories, crop, to produce small-scale quantities of syrup
which has a clean flavor profile and no lingering for local sale, mostly at roadside stands and
bitterness, and it can also be supplied as a pow- farmers markets. However, with consumers
dered extract. Monk fruit extract contains mainly demanding more healthy, non-GMO, and mini-
fructose and glucose, and the sweetness is mally processed sweeteners, in recent years there
972 G. Eggleston et al.
have been developments in the large-scale man- supplement the price support program. In 1988,
ufacture of sweet sorghum syrup, for its reintro- Australia filed a complaint against the United
duction as a commercial liquid sweetener States, charging that the import restriction on
[129]. This endeavor is being backed by the sugar violated the General Agreement on Tariffs
United Sorghum Checkoff Program of the USA. and Trade (GATT) rules. When the United States
Sorghum syrup has a mild caramel taste that has was found to be in violation on some of these
been described as earthy and fruity. rules, it implemented a change from an absolute
quota to a tariff-rate quota. The United States
also has a program called the General System
Regulation and Trade in Sugar of Preferences (GSP) that exempts countries
(mostly in the Caribbean area) from any duty.
Raw cane sugar, refined sugar, sugar syrups, The EU countries import raw sugar within a
specialty sugars, and sugar-containing products special agreement with ACP (Africa, Caribbean,
enter the United States under a variety of tariff- and Pacific) countries.
rate quotas (TRQs). Low within-quota tariff rates Domestic raw cane sugar prices are quoted via
facilitate access to the US market. The minimum the Sugar No. 16 (ICE—Intercontinental
sizes of the TRQs and the corresponding duties Exchange) contract which serves the hedging
reflect obligations made by the United States. needs of US sugar producers, end users, and
When Congress ratified the NAFTA and WTO merchants. The contract prices physical delivery
(Uruguay Round) treaties, these TRQs became of US-grown (or foreign origin with duty paid by
part of the US Harmonized Tariff Schedule. deliverer) raw cane sugar at one of five US refin-
Most of the sugar produced in the world ery ports as selected by the receiver (Simon,
(about 70%) is used for local or domestic con- personal communications). There is no futures
sumption. The remaining 30% is in excess of market for US refined sugar. The world refined
local demand and makes up the global trade in sugar price is based on the Number 5 Contract on
sugar. In recent years, the trend has been toward the London International Financial Futures and
the export of more white sugar instead of raw Options Exchange (LIFFE), which is based on the
sugar. In 2014/2015, the European Union London daily spot market price for refined sugar
exported ~ 1.5 million tons of white sugar. Brazil in free-on-board ships in European ports [132].
is currently the largest exporter of sugar at 24.0 Copies of the Number 11 (world sugar) and Num-
million tons followed by Thailand at 8.5 million ber 14 contracts (domestic) for raw sugar can be
tons and Australia at 3.5 million tons. China found in issues of F.O. Lichts World Sugar and
imports 3.8 million tons sugar while the Sweetener Yearbook prior to 2002.
European Union imports 3.5 million tons and The USDA’s Sugar-Containing Products
the USA 3.1 million tons. Overall, there are Re-Export Program is designed to put US
51.8 million tons of sugar imported while there manufacturers of sugar-containing products on a
are 53.7 million tons exported throughout the level playing field in the world market. The
world [130, 131]. Refined Sugar Re-Export Program is designed to
Trade in sugar throughout much of the world facilitate the use of domestic refining capacity to
is controlled by agreements and special trading export refined sugar into the world market. The
arrangements. The United States regulated sugar program establishes a license against which a
production, distribution, and importation by refiner can export domestically produced refined
means of the Sugar Act of 1948 as amended sugar and later import world raw sugar, import
(US Congress, Public Law 339), but the act was world raw sugar for refining and distribution into
allowed to expire in 1974. From 1981 to the the domestic market, and later export refined
present, the United States has had a price support sugar, or import raw sugar, refine it and export it
program, connected to farm legislation. In 1982, into the world market. The program was
an import quota system went into effect to implemented to mitigate the imposition of
Sugar and Other Sweeteners 973
restrictive quotas, which reduced the quantity of also be linchpins in effective sustainability
raw sugar allowed to enter the US domestic programs.
market.
Because these have been in place for some years, 18. K€ordel P (1998/1999) New equipment and processes
there is more acceptance of the products. in the sugar industry. FO Lichts Guide to Equipment,
Products and Services for the Sugar and Allied
Industries, Directory of Suppliers, pp E3–E25
19. Rein P (2002) Cane preparation. Sugar Bull 8:9–11
20. Ducasse V (1978) Heavy duty chopper fiberiser.
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