Short Report 144
The full version of RIRDC Publication number 07/145 titled:
High-power Ultrasound to Control Honey Crystallisation can be
obtained electronically from RIRDC’s website.
These reports belong to RIRDC’s diverse range of over 1600 research
publications and are part of our Honeybee R&D which aims to
provide knowledge to underpin profitable, sustainable and resilient
agroforestry within Australian farming systems and
landscapes.
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Rural Industries Research and Development Corporation Level 2, 15
National Circuit Barton ACT 2600
Phone: 02 6271 4100 Fax: 02 6271 4199 Email:
[email protected].
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Background It is a common problem within the honey industry for
heat-treated liquefied honey to crystallise during storage,
particularly during cold weather. Since liquid honey is preferred
by Australian consumers, and by food companies (for ease of
handling), then an alternate method to expensive and time-consuming
heating is required to retard the crystallisation process in honey.
Creamed honey production is a difficult process to control,
particularly related to crystallisation, the size of the D-glucose
monohydrate crystals, and thus the quality of the final product
related to hardness and spreadability.
The process used by the honey industry to produce creamed honey is
based on the Dyce method (Dyce, 1931a,b; Dyce, 1976). Ultrasound
treatment has the potential to control this crystallisation
process. However, before any effects of ultrasound can be
determined, it is necessary to be able to produce high quality
creamed honey in the laboratory using the Dyce method, and to be
able to determine the amount of crystalline D-glucose monohydrate
present in creamed honey. Ultrasound treatment was examined to
determine if it can improve the creamed honey process and the
stability of the final product.
This report details the successful development of a process for
liquefying candied honey based on the use of ultrasound technology.
This research is important due to the concern within the honey
industry that the present heating regime used to liquefy candied
honey is reducing the quality of honey, particularly its flavour.
Therefore, it was necessary to undertake this research project to
determine if it was feasible and cost effective to replace the
present heat treatment used by the honey industry for the
liquefaction of naturally crystallised or candied honey, with an
ultrasound treatment. The experiments undertaken used a laboratory
scale ultrasound processor to gather critical data that could be
used to support industrial scale-up trials within a honey packing
company, or by beekeepers. In addition, the Dyce creamed honey
process was examined with respect to the factors that affect the
crystallisation of D-glucose monohydrate and thus the quality of
creamed honey, and whether ultrasound treatment could improve the
quality of creamed honey.
Differential scanning calorimeter
Written by:
Dr Bruce D’Arcy is a food scientist, analytical chemist, and Senior
Lecturer in food chemistry in the School of Land, Crop and Food
Sciences at The University of Queensland. He is Director of the
Australian Honey Research Unit at the University of Queensland, has
extensive knowledge of the physicochemical properties of honey, and
has been researching various aspects of the chemistry, physical
properties and product development of species-specific floral types
of Australian honey for the past 14 years.
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Who is the information targeted at? This report is targeted at
beekeepers and honey packing companies.
Aims and Objectives Aims: (1) To reduce the amount of expensive
heating and loss in quality during liquefaction of candied honey by
developing an alternate, cost-effective ultrasound based method for
the partial or complete liquefaction of candied honey, with a view
to ultrasound having direct application for beekeeper control of
honey crystallisation, or for liquefying candied honey prior to
decanting in a honey packing plant.
(2) To better control the texture of creamed honey spread by
developing an ultrasound based method that enhances the nucleation
rate and produces uniform crystal growth in a creamed honey system,
with a view to it being used by beekeepers and honey processors for
producing consistent and high quality creamed honey.
Objectives: (1) To investigate the effect of ultrasound treatment
on candied honey, including individual glucose monohydrate
crystals
(2) To determine the ultrasound conditions for liquefying candied
honey and for controlling crystallisation in honey
(3) To investigate the effect of ultrasound treatment on the
creamed honey production process
Methods Used 1. Effect of Ultrasound Treatment on the Liquefaction
of Candied Honey The main study of the effect of ultrasound on
candied honey was divided into three experiments.
In the first ultrasound liquefaction experiment, it was necessary
to determine which laboratory scale ultrasound sonotrode, out of
the available 7 mm, 12 mm or 40 mm diameter sonotrodes, better
liquefied candied honey. Candied honey (~250
g) was treated with ultrasound energy interrupted after each of six
10,000 J intervals, for predetermined input energy levels, using
three ultrasonic sonotrodes, with the temperature profile in the
honey being monitored during each interruption. Input energy,
treatment time and power measurements were also recorded from the
ultrasonic processor.
The optimum sonotrode (40 mm diameter) and amplitude (12 µm) were
selected in Experiment 1. The first aim of Experiment 2 was to
determine the minimum input energy required for complete
liquefaction. The use of too high an input energy not only wastes
energy but will unnecessarily increase the temperature and
treatment time. The second aim was to determine if the ultrasound
treatment adversely affected the quality of the honey. The third
aim was to determine the specific energy input (kWh) required to
liquefy one kilogram of candied honey, in order for the developed
novel ultrasound liquefaction method to be useful for the honey
industry. In the second ultrasound liquefaction experiment, candied
Salvation Jane honey samples were treated with six different
ultrasound input energy levels using this optimum sonotrode and
amplitude. These liquefied honey samples were analysed for their
hydroxymethylfurfural (HMF) concentrations, and diastase and
invertase activities, since these three quality parameters are
normally used by the honey industry and regulators to gauge the
heating history and quality of honey.
To complete the ultrasound liquefaction study, a third experiment
was carried out to determine the effect of ultrasound treatment,
relative to heat treatment, on the stability of liquid honey with
respect to subsequent crystallisation on storage. In the third
ultrasound liquefaction experiment, candied reworked mixed honey
(~200 g) was completely liquefied by ultrasound
Ultrasound equipment setup
treatment. Reworked mixed honey was selected for this trial as it
is a very fast crystallising honey that produces large crystals.
This permitted a crystallisation study to be completed in a short
time-frame. Crystallisation of ultrasound-treated honey under
optimum conditions of 14 °C was monitored (using a microscope as
part of an image analyser) and compared with crystallisation in
honey samples initially treated with a standard heat
treatment.
2. Evaluation of the Effect of Ultrasound Treatment on the Creamed
Honey Production Process
A study was carried out to optimise a method to determine the
amount of crystalline D-glucose monohydrate present in creamed
honey, and to produce a laboratory creamed honey with a similar
level of D-glucose monohydrate crystals to that of the commercial
Capilano Honey Ltd. creamed honey. Various honey blends were used
to produce creamed honey using the Dyce method, and the amount of
crystalline D- glucose monohydrate present in these laboratory
creamed honeys was determined using a differential scanning
calorimeter (DSC).
Results/Key findings 1. Effect of Ultrasound Treatment on the
Liquefaction of Candied Honey The main finding from the first
experiment was that the 40 mm diameter sonotrode operated at the 12
µm amplitude was optimum for completely liquefying candied honey.
While it has a lower maximum net power for any 1 s period
during
treatment than does the 22 mm diameter sonotrode, the maximum net
power for the 40 mm diameter sonotrode increased steadily after
each of the six interrupted 10000 J energy inputs as the honey
liquefied, while the maximum net power for the 22 mm diameter
sonotrode initially increased, but decreased markedly from the
fourth 10000 J energy treatment onwards. As the candied honey
liquefies, the power output from the sonotrode increases until the
honey is liquid, at which point there is little increase in maximum
net power. The decrease in net power after an initial increase
observed for the 22 mm diameter sonotrode indicates that there was
poor efficiency in the emission of energy from the 22 mm diameter
sonotrode into the candied honey. The 7 mm diameter sonotrode
produces a lower maximum net power than the other two sonotrodes,
again indicating poor output efficiency of energy from this
sonotrode into the candied honey.
Cumulative treatment times were lower for the 40 mm sonotrode (324
s to 383.3 s; lowest for the 12 µm amplitude) relative to those for
the 7 mm (588.3 s to 681.3 s) and 22 diameter (394.7 s to 871.0 s)
sonotrodes. In addition, the variation in treatment times among
replications was also lower for the 40 mm diameter sonotrode. The
more efficient the emission of energy from the sonotrode to the
honey, the shorter the treatment times. Finally, the maximum
temperature reached after the sixth interrupted 10000 J of energy
input was significantly (P<0.05) lower for the 40 mm diameter
(66.2 °C to 67.8 °C) sonotrode relative to the 7 mm (78.2 °C to
84.4 °C) and 22 mm (76.4 °C to 82.8 °C) sonotrodes. This reflects
the shorter treatment time for the 40 mm diameter sonotrode, which
was possibly due to the high maximum net power produced by
it.
Key Finding: Since treatment times need to be as short as possible
and temperatures as low as possible, then the 40 mm diameter
sonotrodes operated at an amplitude of 12 µm is the optimum
condition for complete liquefaction of honey on a laboratory
scale.
In the next experiment, a preliminary trial showed that a range of
input energies from 50000 J to 70000 J would produce a range of
liquefaction efficiencies from partially liquefied to completely
liquefied. During a replicated trial involving six input energies
between 50000 J and 70000 J, only an input energy of 70000 J
completely liquefied candied Salvation Jane honey. The other energy
inputs only partially liquefied the candied honey. In addition, the
time needed to emit each of the fixed energies from the sonotrode
increased from 304 s for 50000 J of input energy to 434.0 s for
70000 J of input energy, since it takes longer for a sonotrode to
emit more energy. However, there was no significant (P>0.05)
difference in the maximum temperature (which ranged 69 °C to 77.3
°C) after each of the six fixed energy treatments. Further, the
maximum net power recorded at any 1 s interval during each energy
level treatment was not different from each other.
Key Finding: A 70000 J ultrasound energy treatment can be used to
completely liquefy candied honey in a relatively short time of 434
s, without it adversely affecting the maximum temperature generated
in the honey relative to lower energy treatments.
There was no significant (P>0.05) difference in the HMF
concentration in honeys treated with between 50000 J and 62500 J of
input energy and honeys that were heat-treated. However, the HMF
concentrations in the honeys treated with 65000 J and 70000 J of
input energy were
HBE - SR144 Honey Crystallisatio3 3 31/10/2007 1:55:54 PM
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significantly (P<0.05) lower than the HMF concentration in the
heat- treated honeys. This is primarily due to the honey being at
the maximum temperature reached of 77.3 °C for a much shorter time
(434.0 s) than for a heating regime (55 °C for 16 h and 72 °C for 2
min) which is similar to that presently used by the honey industry.
The effect of the energy treatments on enzyme activity was
negligible since there were no significant (P>0.05) differences
in the diastase activity between honeys treated with any of the six
energy inputs and those that were heat- treated, while the
invertase activity of most of the ultrasound treated honey was
higher than the heat-treated honeys, with this difference not
always being significant.
Key Findings: Use of an ultrasound input energy of 70000 J from a
40 mm sonotrode operated at an amplitude of 12 µm is sufficient to
liquefy candied Salvation Jane honey (~250 g) without compromising
honey quality. For example, this ultrasound treatment results in
the production of a lower concentration of HMF from honey sugars ,
and no decrease in diastase and invertase activities, relative to a
heating regime (55 °C for 16 h and 72 °C for 2 min) similar to that
used by industry. The specific energy input needed to completely
liquefy candied Salvation Jane honey is 0.126 kWh/kg. Therefore, 10
kg of candied honey will require 1.26 kWh, while 300 kg will
require 37.9 kWh.
The first finding from the third experiment was that the D-glucose
monohydrate crystallised differently in each type of treated honey.
In the heat-treated honey samples, the initial plate crystals that
formed at between 14 and 28 days were long thin, spiral- shaped
plate crystals. In contrast, in the ultrasound-treated honey
samples, most of the initial crystals that formed at between 14 and
49 days were large pentagon-shaped
plate crystals. In addition, more needle crystal masses were formed
in the heat-treated honeys than were produced in the
ultrasound-treated honeys at the end of the monitoring period of
112 days (16 weeks). Moreover, in heat-treated honeys, plate
crystals grew underneath these needle crystal masses in the later
stages of crystallisation. In contrast, in ultrasound-treated
honeys, plates formed after the needles, with subsequent needles
growing on these initial plates.
Key Finding: Ultrasound treatment delays D- glucose monohydrate
crystallisation more than does a heat treatment similar to that
used by the honey industry. This occurs at both the microscopic
level (in a drop of honey) and in bulk samples. In addition, there
is a difference in the crystal formation process at the microscopic
level in ultrasound- treated honey relative to that in heat-treated
honey. The reason for this is not clear, and requires further
study. Thus, ultrasound treatment will not only liquefy candied
honey without the need for long exposure to high temperatures, but
may make the liquefied honey more stable to subsequent
crystallisation on storage.
2. Evaluation of the Effect of Ultrasound Treatment on the Creamed
Honey Production Process Samples of commercial Capilano Honey Ltd.
creamed honey were initially analysed and found to have an average
crystalline D-glucose monohydrate content of 39.6-40.1 g/100 g
honey. In addition, two blends consisting of 70% alfalfa honey/30%
blue gum honey and 70% canola honey/30% red gum honey were chosen
for a subsequent
Growth of needle crystals in ultrasound-treated honey (identical
view on one slide of one replicate over time)
Growth of needle crystals with time in heat-treated honey
Plate crystal formation within needle crystal masses
HBE - SR144 Honey Crystallisatio4 4 31/10/2007 1:56:06 PM
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Finally, ultrasound treatment was then applied to the seed honey
prior to it being added to the honey blend. The hypothesis is that
if the size of the crystals in the seed honey can be reduced by
ultrasound treatment, then the creamed honey process could be
enhanced (producing a higher level of crystals) and the final honey
would have smaller crystals. This was not the case, and the level
of crystals was not significantly (P>0.05) different from the
control creamed honey produced with seed honey that was not
ultrasound treated. Included in this experiment was the use of
ultrasound treatment of the seeded honey blends at one day and two
days after the addition of the seed honey. Again, such treatments
were hypothesised to reduce the crystal size and enhance subsequent
crystallisation during storage at 14 °C. However, there was no
significant (P>0.05) difference in the crystalline D-glucose
monohydrate content relative to the control untreated creamed
honey. None of the ultrasound treatments enhanced the level of
D-glucose monohydrate crystals relative to the untreated creamed
honey.
Key Finding: The untreated canola/red gum creamed honeys (47.1
g/100 g honey) had similar crystal contents to the
ultrasound-treated canola/red gum creamed honeys (44.5 g/100 g
honey to 47.1 g/100 g honey), while the untreated alfalfa/blue gum
creamed honeys (33.1 g/100 g honey) had similar crystal contents to
ultrasound- treated alfalfa/blue gum creamed honeys (32.2 g/100 g
honey to 33.1 g/100 g honey).
Finally, conditioning of the creamed honey product was
investigated. The reason for this is that some of the creamed honey
samples produced were creamy in texture and some were semi-solid in
texture. There did not seem to be any particular treatment that led
to one type of product over the other. In fact, replicates of the
same treatment often had both types of texture. As part of the Dyce
process (Dyce, 1931a,b; Dyce, 1976), a conditioning step is used
prior to the creamed honey being sent to supermarkets for sale.
Conditioning is where the creamed honey is stored at 30 °C for a
number of days. This study found that such conditioning did produce
consistency in texture with all product having a creamy texture.
The storage at
Image analyser
replicated study, since these produced laboratory creamed honeys
that were soft and spreadable, with crystalline D-glucose
monohydrate contents of 21.6 g/100 g honey (after eight days
storage at 14 °C) and 21.9 g/100 g honey (after 12 days storage at
14 °C) respectively. Alfalfa and canola honeys are fast
crystallising, fine-grained honeys, while blue gum and red gum
honeys have strong flavours. But the level of crystals was not high
enough.
A study was then carried out to increase the level of D-glucose
monohydrate crystals in the laboratory-creamed honey produced using
the above honey blends. One experimental factor that was changed
was the length of storage time at 14 °C, since commercial processes
use 42 days of storage to produce the maximum possible level of
D-glucose monohydrate crystals. When 39 days of storage were used,
a laboratory- creamed honey with a crystalline D-glucose
monohydrate content of 47.1 g/100 g honey was produced, which is
higher than that found in commercial Capilano Honey Ltd. creamed
honey. Thus, the honey blend and creamed honey process had been
optimised in the laboratory.
To further study the creamed honey process, ultrasound treatment
was investigated as a means of reducing the crystal size, and thus
improving the spreadability of the product. Prior to the start of
this project it was thought that ultrasound treatment of the
D-glucose monohydrate crystals in honey would shatter them, thereby
reducing their size. However, the use of an image analyser has
shown that rather than reducing the crystal size through break up
of the crystals, the crystal size is reduced through partial
melting or dissolution of the D-glucose monohydrate crystals. The
clean, sharp crystal structures (plates) are replaced by irregular
shaped plates, indicating that some glucose molecules on the edge
of the crystal structure dissolve into the surrounding liquid,
producing plate crystals that have melted edges and surfaces.
HBE - SR144 Honey Crystallisatio5 5 31/10/2007 1:56:10 PM
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30 °C for 14 days produced a small reduction in the crystalline
D-glucose monohydrate content, with the final content being similar
to that found for commercial Capilano Honey Ltd. creamed
honey.
Key Finding: The conditioning process dissolves some of the D
glucose monohydrate crystals leading to an increase in the amount
of liquid honey, and an overall softening of the creamed honey,
with a consequent improvement in spreadability. While ultrasound
treatment did not produce a product that was different to untreated
creamed honey, conditioning the final product before sale is very
important for producing a consistent product from one production
run to another.
Implications for relevant stakeholders for industry Once the data
from an industrial trial have been obtained, an ultrasound
equipment manufacturing company such as Dr Hielscher GmbH can then
provide specifications for liquefying larger amounts of honey such
as 300 kg in 200 L drums. However, while the time required to
liquefy10 kg or 300 kg of candied honey will depend on the input
power of the ultrasound processor and the capacity of the
sonotrode/sonotrodes, it will be less than the time now used to
liquefy candied honey in hot rooms. The newer, large plastic drums,
which have a completely removable lid, would be ideal for use with
the proposed ultrasound processing system. However, the one
industrial scale problem likely to be encountered relates to the
design of the commonly used 200 L galvabond drums. These drums have
only small openings which, while permitting limited insertion of
the sonotrode, would not permit the moving of the drum up and down
and sideways in a predetermined pattern so as to expose all the
candied honey to the ultrasonic waves. However, as part of the
industrial trials and the subsequent design of the processor
system by an ultrasound equipments manufacturer such as Dr
Hielscher GmbH, such a limitation in the galvabond drums may be
able to be overcome. It is recommended that part of the Australian
honey industry such as major honey packing companies should
undertake these types of industrial trials to ensure technology
transfer from this project to industry.
The results of this study of the Dyce creamed honey process will
aid beekeepers and honey packing companies to better understand
their creamed honey process and improve the quality and consistency
of their product from batch to
batch.
Recommendations Honey packers must make use of this collected data,
by taking up the challenge (and rental costs) of participating in a
scaled-up industry trial involving an industrial ultrasound
processor (much more powerful than used in this project) for
liquefying 10 kg candied honey in commonly used plastic
containers
(e.g. diameter of 270 mm and height of 240 mm). This would be done
in consultation with an ultrasound equipment manufacturer such as
Dr. Hielscher GmbH and the project’s research team. As part of the
recommended system design, the ultrasound sonotrodes will have to
be inserted into the drum to a particular depth in order to liquefy
the honey down to the bottom of the drum. Initially, the sonotrode
will be in contact with the hard candied honey near the top of the
container. As liquefaction of the surface candied honey proceeds,
the honey container will need to be moved upwards and sideways in a
predetermined pattern, so that the sonotrode is brought in contact
with as much of the candied honey as possible, so as to minimise
the treatment time required. In addition, or alternatively, a
stirrer could be inserted in the semi- melted honey to mix the
liquid honey with the remaining candied honey, thereby creating a
flow in the container past the treatment region around the
sonotrode. Ultrasound waves dissipate quickly at a short distance
from the sonotrode, so some mixing is required.
HBE - SR144 Honey Crystallisatio6 6 31/10/2007 1:56:12 PM
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