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Marasinghege, Chalani, Rackemann, Darryn, & Doherty, William


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Assessment of pH control strategies to minimise sucrose losses during
juice evaporation in raw sugar manufacture.
In Proceedings of the 43rd Annual Conference of the Australian Society of
Sugar Cane Technologists (ASSCT 2022).
Australian Society of Sugar Cane Technologists - ASSCT, Australia, pp.
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Peer-reviewed paper

Assessment of pH control strategies to minimise


sucrose losses during juice evaporation in raw sugar
manufacture

Chalani Marasinghege, WOS Doherty and DW Rackemann

Queensland University of Technology, PO Box 2434 Brisbane 4001, Australia;


chalani.marasinghe@hdr.qut.edu.au, d.rackemann@qut.edu.au

Abstract During juice evaporation sucrose loss can occur as a result of degradation reactions that are
catalysed by heat, pH and other juice components. The impacts of heat and juice quality can be
controlled through process and equipment design. Potential pH control strategies for juice were
assessed to minimise sucrose degradation and the subsequent impacts on downstream
processing during the sugar manufacturing process. These strategies were: (1) the use of
reagents to improve the buffering capacity of the juice; (2) the use of neutralising alkanolamines;
and (3) on-line pH adjustment during juice evaporation to minimise pH drop. All these strategies
achieved significant reductions in sucrose loss of 20-50% in both the small-scale and laboratory
rig trials but some come at the expense of chemical costs and other processing implications such
as scaling of the evaporators. The use of ammonia was the preferred pH control strategy,
although it led to an increase in juice colour.

Key words Sucrose loss, buffering reagents, neutralising amines, pH control, evaporation

INTRODUCTION

The evaporation station is the most energy-consuming operation during raw sugar manufacture. Processing
changes in the evaporators are typically used by sugar factories to improve energy efficiency. These changes
include installation of additional heating surface area and evaporation capacity. Unfortunately, they lead to longer
juice-processing times in the evaporators, which increase the chemical degradation of sucrose (and invert) and the
formation of acidic products in both the juice and condensates. One of the consequences is increased corrosion
of the evaporator equipment (Eggleston et al., 2019; Eggleston & Monge 2007; Rackemann & Broadfoot 2016,
2017; Cox et al. 1993).

During evaporation, loss of sucrose is caused by acid-catalysed hydrolysis to glucose and fructose, and this loss
can be >1% in factories employing extensive vapour bleeding at the front end of the evaporator set because of
higher juice temperatures and longer residence times (Rackemann & Broadfoot 2016). Up to 80% of the sucrose
loss occurs across the first two effects (Rackemann & Broadfoot 2017). Along with increasing sucrose losses, a
decline of juice pH (and hence increase in juice acidity) is observed, which is due to the degradation of invert into
organic acids, volatilisation of ammonia (produced from proteins and amino acids degradation) from the juice to
vapour stream, and deposition of acidic scale compounds on the heated tubes (Edye & Clarke 1995; Eggleston &
Amorim 2006).

Reductions of juice residence times and the lowering of juice temperatures are some of the strategies to minimise
sucrose degradation, but these require substantial capital investment and affect process efficiencies (Rackemann
& Broadfoot 2016). Eggleston & Monge (2005, 2007) have reported that operating at higher juice pH than that
required to achieve good clarification is the simplest solution to minimise sucrose losses in evaporators. However,
careful consideration should be given to the appropriate pH value as high juice pH brought about by increased
saccharate addition will increase the level of scaling in the evaporators which overrides some of the benefits. High
juice pH also increases invert sugar degradation and so will also have a negative impact on raw sugar quality
(Eggleston 1998; Eggleston & Lee 2018). Invert degradation products consist of both coloured and acidic products,
and these will further lower the pH of the juice during the evaporation process. Some of these acidic degradation
products will volatilise into the vapour streams and cause condensates to have lower pH values (Rackemann &
Broadfoot 2016). The pH drop over the course of the evaporation process will further cause sucrose degradation
and, hence, further losses.

Here, we assessed potential pH control strategies for juice for their ability to minimise sucrose degradation and the
subsequent impacts on downstream processing during the sugar manufacturing process. These strategies (Figure
1) were: (1) the use of reagents to improve the buffering capacity of juice and so minimise pH drop; (2) on-line pH
adjustment during juice evaporation to minimise pH drop in the juice; and (3) the use of neutralising alkanolamines.

Figure 1. Approaches used for the study and expected outcomes.

EXPERIMENTAL
We conducted thermal degradation tests of ESJ solutions at 120 °C using sealed 30 mL glass pressure reactor
tubes heated in an oven or by boiling larger volumes of ESJ solutions in a laboratory evaporator-condenser rig.
For the oven tests, samples were prepared in duplicate, sealed with screw caps and placed in an oven pre-
equilibrated at 120 °C and heated for 75 min to simulate thermal degradation that occurs in evaporators. The tubes
were then placed in an ice bath to cool to room temperature, followed by pH measurement and analysis for sugars,
organic acids, and minerals to determine sucrose losses and other changes in juice composition.

For the laboratory rig boiling tests (Figure 2), a volume of 4.5 L of ESJ, collected from Rocky Point Sugar Mill (pH
7.7, 11.0 Bx and sucrose/brix of 94.7%), was boiled in the rig at 119.5 °C for 60 min while the silicon oil temperature
was 148 ± 0.5 °C to maintain a constant heating temperature differential. The time taken for the solution to initiate
boiling was ignored, and the time at which juice started boiling was marked as the start of the test (t=0 min).
Sampling points were available to collect juice and returning condensate samples. Vented vapour was condensed
and collected throughout the test and at the end of the test period. All samples were immediately cooled to room
temperature using an ice bath, and the pH of all samples and the brix of juice samples were measured at ambient
temperature prior to storage at -20 °C for further analysis.

Description of the laboratory rig

The rig (Figure 2) consists of a jacketed evaporator vessel with an internal heating coil through which silicone oil is
circulated to heat the juice. The juice boiling temperature is controlled by setting the evaporator vessel headspace
pressure (i.e. 100 kPa.g). The vapour produced by evaporation of the juice passes through the condenser, and
the condensate is returned to the juice in the evaporator vessel. Vapour vented from the apparatus to regulate the
pressure is separately condensed.
Figure 2. Flow diagram of the laboratory rig used to mimic a factory evaporator.

Buffering reagent tests

The buffering capacity of ESJ with and without addition of reagents was first determined. The regents we used
were trisodium citrate and disodium hydrogen phosphate (Na 2HPO4). The buffering capacity curve of ESJ was
determined by titrating a volume of 50 mL ESJ (with and without adding the buffering reagents) against 0.2 M HCl
or 0.2 M NaOH solutions at 20 °C according to method described by Salaün et al. (2005). The volume of titrant
used for every 0.10 unit pH change of the solution was noted and the buffering capacity (dβ/dpH) was calculated
using the following equation.

𝑑𝛽 (𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑜𝑟 𝑏𝑎𝑠𝑒 𝑎𝑑𝑑𝑒𝑑) × (𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑜𝑟 𝑏𝑎𝑠𝑒)


=
𝑑𝑝𝐻 (𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒) × (𝑝𝐻 𝑐ℎ𝑎𝑛𝑔𝑒 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑)
(1)

Calculated dβ/dpH values were plotted against pH of the solution to determine the pH at which ESJ shows
maximum buffering capacity.

Thermal degradation tests were conducted by adding a known mass of buffering additive (Na 2HPO4, trisodium
citrate) dissolved in 10 mL of ESJ solution placed in a pressure reactor tube. The pH of the solution was measured
at room temperature. A control test with ESJ without any buffering additive was adjusted to the same pH as the
test solutions using a 10% Ca(OH)2 solution.
Neutralising amine tests

Alkaline amines were used to raise the pH of both the ESJ juice and condensates. The neutralising amines tested
in the laboratory rig were cyclohexylamine, monoethanolamine, 3-methoxypropylamine, 2-diethylaminoethanol,
morpholine and ammonia. At the initiation of boiling, a quantity of amine equivalent to 3 mM was dissolved in 10
mL of ESJ and was injected into the evaporator vessel headspace, followed by a volume of 40 mL of ESJ to flush
the injection line. Juice sampling was undertaken at 20 min intervals, and the returning condensate was sampled
at 10 min intervals and the total amount of vented vapour was collected at the end of the test. Randomised
experiments were conducted in duplicate to determine repeatability and the variation among tests.

On-line pH control tests

On-line pH control tests were also conducted in the laboratory boiling rig. A volume of ~1 mL of 10% Ca(OH)2 or
28% ammonia followed by 10 mL of ESJ was injected into the boiling juice in the rig at 10 min time intervals within
the 60 min boiling period to maintain the juice pH. As a comparison, a control test was conducted without any
spiking of alkaline solution, but with 10 mL of ESJ added at intervals. Juice sampling was undertaken every 20 min,
returning condensates were collected at 10 min intervals and final vent condensates were collected at 60 min for
analysis.

Analytical procedures

pH and brix of composite juice samples were measured onsite at the completion of each sampling test. pH was
measured using a temperature-compensated portable handheld Seven2Go pH meter (Mettler Toledo). The brix at
ambient temperature was measured using a handheld digital refractometer.

Sucrose, glucose, and fructose were measured according to the official ICUMSA Method GS7/8/4-24 (1998) by
High Performance Ion Chromatography (HPIC) using pulsed amperometric detection.

Sucrose losses or degradation were measured based on the Glucose % Sucrose method (Schaffler et al., 1985)
given by:

%𝐺𝑙𝑢𝑐𝑜𝑠𝑒𝑓𝑖𝑛𝑎𝑙 %𝐺𝑙𝑢𝑐𝑜𝑠𝑒𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑀𝑊𝑠𝑢𝑐𝑟𝑜𝑠𝑒


𝑆𝑢𝑐𝑟𝑜𝑠𝑒 𝑙𝑜𝑠𝑠 (%) = − × × 100
%𝑆𝑢𝑐𝑟𝑜𝑠𝑒𝑓𝑖𝑛𝑎𝑙 %𝑆𝑢𝑐𝑟𝑜𝑠𝑒𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑀𝑊𝑔𝑙𝑢𝑐𝑜𝑠𝑒
(2)

Alternatively, sucrose degradation was also measured by calculating % Sucrose loss (mass basis) as:

𝑆𝑢𝑐𝑟𝑜𝑠𝑒𝑖𝑛𝑖𝑡𝑖𝑎𝑙 −𝑆𝑢𝑐𝑟𝑜𝑠𝑒𝑓𝑖𝑛𝑎𝑙
𝑆𝑢𝑐𝑟𝑜𝑠𝑒 𝑙𝑜𝑠𝑠 (%) = 𝑆𝑢𝑐𝑟𝑜𝑠𝑒𝑖𝑛𝑖𝑡𝑖𝑎𝑙
× 100 (3)

Organic acids were determined by a modified High Performance Liquid Chromatography (HPLC) method of Blake
et al. (1987).

Colour of juice samples adjusted to pH 7.0 was measured as the absorbance at 420 nm and calculated according
to the official ICUMSA method OS2/3-9.

For the measurement of mineral concentration of juice samples, juice samples diluted to a specific ratio were spiked
with 200 µL of highly concentrated distilled nitric acid and analysed using Inductively Coupled Plasma Optical
Emission Spectrometry (ICP-OES).

Total N content of vent and condensate samples diluted to a specific ratio were determined using a Shimadzu
TOC-V TN instrument.

Analyses were completed in duplicate. Standard errors of sucrose losses, organic acids concentration, minerals
concentration and N levels were ±0.1%, ±7.1 ppm, ±35.7 ppm and ±5.0 ppm, respectively.
RESULTS AND DISCUSSION

Buffering reagents

Sugarcane juice contains sugars, organic acids, polysaccharides, amino acids, and non-nitrogenous acids such as
phenolics in equilibrium with their ionic forms, and thus can be considered as a buffer solution (Arif et al. 2019;
Holkem et al. 2019). The buffering action of sugarcane juice is mainly attributed to the presence of aconitic acid in
the juice which accounts for two-thirds of all the organic acids in the juice (Arif et al. 2019), while all the other acids
and bases also contribute to the buffering to a smaller extent. The pH of natural sugarcane juice usually lies
between 5.2 to 5.4 units.

Figure 3 shows the variation of the buffering capacity (dβ/dpH) against pH at 20 °C after adding reagents to raise
the pH of ESJ from 7.0 to 7.4. The concentration of trisodium citrate and Na2HPO4 added to raise the pH was
8600.4 and 5260.0 ppm, respectively, while pH of the control solution was raised by adding 10% aqueous Ca(OH) 2
equivalent to 220.0 ppm as Ca(OH)2 or 120.0 ppm as Ca. The maximal buffer capacity regions represent the pHs
at which the juice shows strongest resistances to pH changes when H + or -OH ions are added. Existence of multiple
peaks in buffering regions may be due to the occurrence of different types of weak acidic and basic moieties in
sugarcane juice. In the control ESJ solution, no buffer capacity was observed between pH 7.0 and 7.8, in the
region expected for ESJ (Figure 3). As shown in Figure 3, the maximal buffer capacity with Na 2HPO4 was in the
pH range of 6.0 to 8.0 corresponding to its pKa (7.21) and that of trisodium citrate lies in the range of 4.0 to 6.0
corresponding to its pKa (4.74). So, from this acid-base adjustment tests of ESJ, Na2HPO4 shows the highest
buffering capacity.

Figure 3. Buffering capacity of ESJ when acidified and alkalinised respectively with 0.2 M HCl and 0.2 M NaOH
with and without buffering additives.

To determine how these reagents would respond with boiling ESJ, juice samples (pH 7.7) with and without
treatment with the buffering reagents were boiled in the glass pressure reactor tubes and heated in the oven at
120 °C for 75 min to determine pH drop and compositional changes (Table 1). As there were less pH drop observed
for the ESJ solutions with the buffering reagents, lower sucrose losses compared to the control are expected. The
sucrose losses calculated using the glucose/sucrose ratio of Equation 2 gave losses 0.86%, -0.54% and -0.15%
for the control, Na2HPO4 and trisodium citrate respectively. The negative losses obtained with the reagents are
due to higher glucose degradation compared to glucose formation resulting from sucrose hydrolysis compared to
the control. Tests with glucose alone showed that the two buffering agents isomerised some of the glucose to
fructose. As the brix of the samples remained constant during the course of the experiments, sucrose losses were
determined by calculating % sucrose loss using Equation 3. Results of 2.29%, 1.47% and 1.52% for the control,
Na2HPO4 and trisodium citrate tests respectively were obtained. Measuring the sucrose loss in this way is reliable
for these set of experiments as there were no losses in volume throughout the test period.
Table 1. Juice composition obtained with and without treatment with buffering reagents.

Test Control Na2HPO4 Trisodium citrate


Time (min) 0 75 0 75 0 75
Amount added (ppm) - 8038.2 20216.7
pH (20 °C) 7.65 6.16 7.64 6.94 7.62 6.58
pH drop (%) - 53.0% 30.2%
Brix (20 °C) 14.0 14 14.8 14.6 15.8 15.8
Glucose (kg/kg) ± 0.005 0.200 0.255 0.201 0.160 0.197 0.184
Fructose (kg/kg) ± 0.004 0.216 0.234 0.208 0.136 0.223 0.162
Sucrose (kg/kg) ± 0.024 13.356 13.051 13.328 13.132 13.148 12.948
Glucose/Fructose 0.93 1.09 0.97 1.18 0.89 1.14
Sucrose loss (%)
Glucose / Sucrose (Eqn 2) 0.86 -0.54 -0.15
% Sucrose loss (Eqn 3) 2.29 1.47 1.52
Organic acids (ppm)
Oxalic acid 22.1 22.3 29.7 28.0 n.d. n.d.
cis-Aconitic acid 41.7 77.2 41.0 51.8 37.8 49.5
Citric acid 93.9 89.3 n.d. n.d. 6490.9 6793.5
D-Gluconic acid 44.4 41.7 36.2 69.0 n.d. 7.5
L-Malic acid 86.5 78.5 80.3 87.8 15.4 13.1
trans-Aconitic acid 494.1 426.4 446.2 439.3 407.8 407.0
Succinic acid 17.5 15.5 n.d 5.3 n.d. n.d.
L(+)-Lactic acid 54.1 50.9 n.d. 2.3 n.d. n.d.
Formic acid 20.1 41.0 10.4 23.5 3.7 13.8
Acetic acid 54.2 68.1 n.d 12.5 0.9 0.5
Methanol n.d n.d. n.d. n.d. 48.1 85.4
Ethanol 13.2 13.1 17.2 20.4 26.9 33.1
Minerals (ppm)
Ca 309.1 312.0 140.4 143.9 298.3 279.9
K 984.5 974.8 1241.9 1209.3 1367.5 1313.7
Mg 218.9 221.1 158.6 154.8 226.5 213.9
Na 26.8 27.2 2509.7 2436.5 4649.6 4400.3
P 18.5 18.7 1711.0 1686.5 19.3 18.2
S 305.4 305.0 310.2 300.8 319.2 296.9
Si 29.9 41.0 31.2 49.1 29.4 54.2
Overall, the results show that the selected reagents increased juice buffering capacity, and therefore reduced pH
drop and sucrose losses. The sucrose losses observed in these results are much higher than losses reported in
factory trials (Rackemann & Broadfoot 2016; Rackemann & Broadfoot 2017). This is not unexpected as the juice
was boiled for 60 min at ~120 °C whereas the juice boiled in the first effect of cogeneration factories typically only
has a residence time of 20 min or less. There are also other differences between the batch operation in the lab rig
and continuous operation in factories that were outline by Marasinghege et al. (2020). However, the lab rig provides
trends and relative magnitudes for the changes in test conditions and so the results have relevance to factory
operation.

However, the reagents increased the ash content of juice, specifically Na + ions which may be detrimental in
subsequent processing stages due to their melassigenic nature. Addition of Na2HPO4 also caused precipitation of
Ca-phosphate complexes in the juice that will increase fouling propensities on the heating surfaces of the
evaporators. Also, the addition of trisodium citrate increased citrate ion concentration in the juice; the implication
of this is unknown, but as citrate ions are chelating agents they will complex with calcium and perhaps form calcium
citrate scale in the crystallisation pans. The addition of buffering additive has caused some reactions (precipitation
or conversion) with oxalic, citric, succinic and lactic acids resulting in these acids not being identified in the mixture
after the initial heating period (Table 1). The dosages of the reagents required to minimise sucrose loss were high
and so are not cost-effective. If cheaper buffering agents are available, they should be evaluated.

Neutralising amines

Treatment with volatile alkanolamines to raise condensate pH and prevent corrosion is a common treatment
method in several industries such as fossil and nuclear power generation systems and steam generation systems
in food industry (Ahmad 2006; Balakrishnan 1978; Memarzadeh 2014). Here, juice treatment with volatile amines
was conducted to increase the pH of the acidic condensates and to maintain the pH of the juice.

A series of tests were conducted by injecting the neutralising amines to boiling ESJ solutions (Figure 4). The
average pH of the ESJ was 7.7 and 10% Ca(OH)2 solution was added to adjust the ESJ pH to the same value as
the control sample. The sucrose losses (using equation 2) of all amine trials except with morpholine were
substantially lower than the value obtained with the control (Figure 4A), which ranged from 0.66-0.92% during the
60 min boiling period. This accounted for 15-40% sucrose reduction compared to the control. The average juice
pH drop of the control test was about 1.96 units, while the values for the amines were between 1.61-1.86 units.
Cyclohexylamine produced the lowest juice pH drop, and the lowest sucrose loss.

Figures 4B and 4C show the variation of condensate pH of the amines with boiling time. The average condensate
pH of the control dropped from 7.45 to 7.17, while the average pH of the entire vent condensate collected was
7.78. The slightly alkaline pH of the control’s vent condensate could be attributed to the quality and buffering
capacity of the juice that may have contained relatively higher levels of nitrogenous compounds that break down
to form ammonia. Among the amines, cyclohexylamine showed the highest condensate pH over the course of
experimental period, which could be due to its relatively higher volatility or vapour to liquid (V/L) ratio (4.7:1)
compared to the other alkanolamines. The ammonia test recorded the highest pH of the vent condensate samples,
14% higher than that of the control test and is attributed to the low boiling point (-33.3 ⁰C) and higher V/L ratio
(10:1) of ammonia. The lowest condensate pH was recorded by monoethanolamine, but this test showed
surprisingly high pH of the vent condensate. Overall, under the conditions tested, 3-methoxypropylamine and 2-
(diethylamino)ethanol were least effective. While the efficacy of 2-(diethylamino)ethanol could be attributed to its
higher boiling point limiting its volatility, the lower pH exhibited by 3-methoxypropylamine is unexpected as its
boiling point is exceeded under the experimental conditions used. Although morpholine showed high vent
condensate pH, the pH of the condensates during this trial was low. Morpholine is generally recommended for
treating short path condensate systems. Therefore, it is likely that the majority of the morpholine volatilised early
in the experiment making the vent condensate relatively basic leaving a smaller proportion circulating in the
condenser system. In summary, cyclohexylamine and ammonia were the most effective amines.

The major limitation in applying amines (excluding ammonia) to juice and condensate systems is the amount
allowable by the US Food and Drug Administration (FDA). Therefore, selected tests that exhibited better
performances on the condensates’ pH were analysed for their N levels as the amines contain N. To eliminate
interferences by the endogenous nitrogen compound, the vapour from volatilised sugarcane juice condensate
samples from control tests were also analysed for their N levels (Figure 4D). A simple N mass balance for
cyclohexylamine derived condensate showed that out of 299.1 mg of cyclohexylamine added, 101.1 mg circulated
in the condensate system and 40.9 mg was vented and accumulated in the vent condensates, while the rest of the
amine stayed in the juice. The concentration translated to ~ 377.6 ppm of amine in condensates, which is >37
times greater than FDA approved concentration limits. Therefore, despite the efficacy of cyclohexylamine, it is not
considered suitable as a neutralising amine. Thus, ammonia is the preferred neutralising amine that needs further
evaluation.

Figure 4. Results of boiling tests conducted by injecting amines A) Sucrose losses with different neutralising
amines B) Variation of returning condensate pH during the boiling period C) Variation in vent condensate pH D)
Variation of condensate N levels of selected tests.

While greater accumulative benefit would be achieved if low pH conditions are remedied earlier in the evaporator
set, it is noted that amine addition has not been investigated for the end of the set where severe corrosion problems
are also known to exist. Indeed, there may be merit that amine addition could provide a possible remedy to
corrosion problems experienced towards the end of the set.
On-line pH control

The laboratory evaporator rig was used to investigate on-line pH control as a potential strategy to minimise sucrose
losses. In these tests, known amounts of Ca(OH)2 or NH3 was injected to the boiling juice at 10 min intervals to
maintain the juice pH roughly at ~7.3 for the test throughout the 60 min period. In contrast, to Ca(OH)2 treated
ESJ, the control had no pH control and the juice pH reduced to 6.0 after 60 min. The average condensate pH was
~7.7 for both tests. The measured sucrose loss based on the Glucose % Sucrose method (Figure 5) shows that
maintaining the pH over the 60 min period reduced the overall sucrose loss by ~50%, with the extent of loss
compounding over time.

Figure 5. A) Measured sucrose loss and B) pH change during ESJ boiling with continuous adjustment of pH to
~7.25 using Ca(OH)2.

Although this approach was effective, the quantity of extra lime added, being equivalent to ~120 ppm of Ca 2+ ions
on juice, is high. Therefore, another alkaline agent, ammonia was trialled under similar conditions, and the results
are shown in Figure 6. Similar to the tests using Ca(OH)2, juice pH was maintained at ~7.25 throughout the 60 min
boiling period where a total of 56 ppm ammonia on juice was dosed, while the pH of the control dropped to 6.0
(Figure 6B). As shown in Figure 6A, pH control by ammonia reduced sucrose loss by ~34% compared to the
control.

The condensate pH derived from ammonia shows increases (after an initial dip) with time in contrast to the control
which decreases with time (Figure 6C). The control-derived vent condensate had a pH of 7.78, while ammonia-
derived vent had a higher vent condensate pH of 8.37. These results suggest that use of ammonia over Ca(OH)2
is more effective to raise the vent condensate pH, and there is a lower risk of fouling of the evaporators. However,
ammonia does contribute to colour development. Colour measurements (at pH = 7.0) showed that the control and
ammonia tests increased colour by 8.1% and 14.1%, respectively. From the results, on-line pH control particularly
with ammonia appears to offer a simple and promising strategy to reduce sucrose losses. It is recommended that
the juice derived from ammonia should be processed to sugar to determine the impact on sugar colour. In addition,
trials with NaOH to control juice pH should be conducted as its use is expected not to affect scaling of the
evaporators, and not have an impact on juice colour as compared to ammonia. The dosage needed to adjust the
juice pH with NaOH will be lower than Ca(OH)2, and so it is expected that it will not impact on sucrose recovery. It
should be noted that significant sucrose losses occur in the early effects, and in steam efficient factories >70% of
the sucrose loss occurs there (Rackemann & Broadfoot 2016). Hence, the dosage of the chemical required for pH
control may be far less than the values reported here. Thus, the application of online pH control would need to be
tested at a factory scale to better quantify the magnitude of the potential benefits.
Figure 6. A) Measured sucrose loss B) pH change during ESJ boiling and C) pH of returning condensates with
continuous adjustment of pH to ~7.25 using ammonia.

CONCLUSIONS
Our study assessed different strategies to minimise sucrose losses during evaporation via pH control. pH control
strategies included the use of buffering reagents, neutralising amines, and on-line pH control using lime and
ammonia. The use of buffering reagents reduced the pH drop of juice and sucrose loss by 33-35% compared to
when they were not used. However, the practical usage of these reagents is limited because of high cost, risk of
melassigenic activity and impacts associated with their interactions with juice constituents. Our results highlighted
the shortcoming of the Schaffler method, that being glucose stability, when using glucose to sucrose ratios for
measuring sucrose losses, as the buffering additives were shown to react with glucose and lead to erroneous
results with this method. The use of neutralising amines to a set pH value was shown to reduce sucrose loss and
raise condensate pH. However, they are prohibited (except ammonia) based on their required addition rates which
exceed FDA guidelines. On-line pH control with ammonia shows promise, but its impact on the quality of the sugar
product should be evaluated as it slightly increases juice colour. It is also recommended that NaOH should be
trialled as its addition will not increase scaling of the evaporators, and because it is of higher alkalinity than either
Ca(OH)2 or ammonia, the amount required for pH adjustment will be relatively small. At the required dosing level,
it should not impact on sucrose recovery.

ACKNOWLEDGEMENTS
The work presented in this paper is based on a PhD program that is part of Sugar Research Australia Limited
(SRA) project 2017/007. Funding provided by SRA is acknowledged. This work was enabled by use of facilities
at the Banyo Pilot Plant Precinct. Neil McKenzie (QUT) is acknowledged for his assistance with the construction
and operation of the laboratory evaporator rig. Rocky Point mill are also acknowledged for providing ESJ samples
used in the investigation.

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