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Determination of
Sugar in Food &
Beverages
Refractometry
Density
Titration
Moisture Analysis
Content 2
1 Introduction 3
2 Solutions Overview 4
3 Efficient Sugar Content Determination in Food and Beverages 4
3.1 Brix Determination with Instruments 4
3.2 Beverages, Juices, Wine 6
3.3 Molasses and Syrups 6
3.4 Multiparameter System with LiquiPhysics Instruments 7
4 Titration of Reducing Sugar 8
5 Moisture and Sugar Content in Sugar 9
5.1 Moisture Determination in Sugar 9
5.2 Water Determination of Raw Sugar 10
6 Production Process Control 12
6.1 Purification Process Monitoring by Titrimetric Analyses 12
6.2 Typical Analyses 12
6.3 Automated Titration System 13
6.4 Advantages 13
6.5 Tips and Hints 13
7 Conclusions 14
8 More Information 15
9 Appendix 15
Sugar
Sugar is the general term for a class of sweet-flavored substances used as food. There are various types of
sugar derived from different sources. Monosaccharides are simple sugars and include glucose, fructose and
galactose. The table or granulated sugar most customarily used as food is sucrose, a disaccharide. Other
disaccharides include maltose and lactose. Table sugar has the chemical formula of C12H22O11, its energy content
is 16.8 kJ per gram, and is heavier than water, with a density of 1.6 g/cm3. The word 'sugar' originates in the
Sanskrit word 'śarkarā', which means sweet; this word was later taken into Arab and from there entered the
European languages.
Sugars are present in sufficient concentrations for efficient extraction in sugar cane and sugar beet. Sugar cane
is a giant grass and has been cultivated in tropical climates in the Far East since ancient times. Sugar beet is a
root crop and is cultivated in cooler climates. Sucrose as a substance is directly contained in these plants and
is extracted in a watery solution by leeching, boiling or pressing and crystallizes in the process of boiling out the
water content. Sucrose is the parameter that is mostly tested in food labs.
The oldest findings of sugar cane in Melanesia, Polynesia, date back to 8,000 b.C.. Around 600 a.D. hot sugar
cane juice was filled into wooden or earthen cones – the creation of the sugar cone. Initially, sugar was a much
sought after substance in Europe and considered a luxury good and medicine. No surprise that sugar was called
the white gold.
In 1747 Andreas Sigismund Marggraf discovered the sugar beet and in 1801 the chemist Franz Carl Achard
created the basis of industrial sugar production. Sugar started to become an industrial commodity and prices
decreased, with the beginning of industrial production from 1850 onwards. An interesting side note: In 1840 the
first sugar cubes were developed. These were initially colored red, as the wife of the developer Jacob Christoph
Rad, who had hurt herself while trying to break some pieces off a sugar cone and had asked her husband to
produce smaller portions. He invented the sugar cube press and colored the first cubes red, in remembrance
of the event. That his wife had still offered the blood-stained sugar to her guests shows the high value it had at
those times.
The world produce of sugar was about 168 million tons in 2011. Top sugar producing countries are Brazil, India,
China, USA and Thailand. The average person consumes about 24 kilograms of sugar each year, equivalent to
over 260 food calories per person, per day. It is not surprising that the increase in sugar consumption (about
20fold in the last 150 years) also had adverse effects on our health. Sugar is thought to have played a major
role in the increase in adiposity, and, as an easy-to-digest carbohydrate has strong effects on the insulin levels.
Inverted sugar is a mixture of glucose and fructose. It is made out of the disaccharide sucrose in a hydrolytic
reaction, which is commonly induced either by the addition of acid, or utilizing sucrases, biological catalysts. In-
verted sugar has some desirable properties: It is sweeter than sucrose, does not crystallize as easily and builds
smaller crystals. Invert sugar also has a lower water activity than sucrose and thus provides for more preserving
qualities. It is hence often utilized by bakers and food producers.
Analytical balance
Moisture analyzer
Precision balance
Moisture content
Refractometry
Water content
Karl Fischer
Weighing
Weighing
Titration
Titration
Density
Food and ingredients
Beverages / Juices
Syrups, molasses, extracts
Sugar as raw material/ingredient
Modern digital refractometers are easy to use and allow the refractive index of liquids to be determined with
a high degree of accuracy. The result is evaluated automatically, indicated on the display, printed or stored.
Temperature is kept constant with built-in solid state thermostats obsoleting water baths.
In addition, the refractive index value can be automatically transformed to Brix or other concentration units
applying the respective conversion tables.
To master high sample throughput, digital lab refractometers are combined with automatic sample changers.
The sample changer also undertake the automatic rinsing and drying of the prism. There is nothing else for the
operator but to place the sample vials on the sample changer and to start the analysis.
Density g/cm3
Temperature ºC
Automatic density meters, applying the measuring principle of the oscillating U-tube, need a few mL of sample
only which facilitates sample procurement considerably. Temperature adjustment and equilibration of the sample
is achieved by the built-in thermostat and controlled by the density meter. Temperature equilibration is achieved
very fast. Thus, density determination including calculation of Brix or other concentration units is shortened to
merely few minutes.
Figure 2: Schematic of density measuring cell with oscillating U-tube and Peltier element for heating and cooling
Conversion Tables
Density and refractive index values can easily be converted into concentration units with the help of conversion
tables. For sugar, density and refractive index are translated into Brix units. Modern instruments automatically
do so. They also compensate to a Brix value at 20°C, if the measurement was conducted at higher temperature.
Thus, manual conversions and erros are avoided.
Because density and refractometers do not specifically determine the sugar content but just the physical property
of a liquid, correlations between density or refractive index data and the respective concentration have been
setup for various compounds e.g. sucrose, HFCS 42 or HFCS 55 (HFCS high fructose corn syrup). Thus, several
conversion tables are available to calculate Brix from refractive index or density values. It is important to apply
the right table to avoid erroneous transformation.
Beverages: Soft drinks such as ice tea,lemonades, syrups and other beverages usually do not require any
sample preparation. Just fill the U-tube of the density meter with a syringe, drop a few drops on the prism of the
refractometers or place the sample vials on the sample changer.
Carbonated beverages: Carbonated beverages need degassing prior to the density determination, because gas
bubbles interfere with the measurement technique of the oscillating U-tube. Dissolved carbon dioxide gas also
contributes to the density, thus falsifying conversion to Brix or other concentration units.
However, carbon dioxide influences the refractive index determination to a much lesser extent. Just ensure that
free bubbles do not collect on the surface of the measuring prism.
Fruit juices: Fruit particles (pulp) can make fruit juice samples inhomogeneous. Thus, pulp needs to be removed
before determining density or refractive index. However, the refractive index determination is less sensitive to
pulp particles than the density determination.
The acid corrected Brix value takes into account the influence of fruit acids e.g citric acid, on the refractive index.
This correction asks for a prior acidity determination (titration, see Acidity Guide) and can then be done rather
easily.
Wine: Red and white wine do not require extended sample preparation but can be directly applied to density and
refractometers.
Density and refractive index are frequently determined in the same sample. Increasingly, more parameters
such as pH value or color are requested. The combination of LiquiPhysics Density and Refractometers,
sample changers and additional insturments provides unparalleled solutions for simultaneous multiparameter
determinations.
Figure 3: Multiparameter system with density and refractometer combined with pH meter, sample changer and LabX software.
* LIMS Laboratory information and management system, ERP Enterprise resource planning systems
The Method
Any sugar having an aldehyde group or is able to form one in solution is a reducing sugar. Typical examples are
aldoses such as glucose, galactose, mannose or xylose. The titration of reducing sugars according to Rebelein
applies to fruit juices, wines and other sugar containing food and beverage products. Hereby react the reducing
sugars with alkaline copper (II) sulfate to form copper (I). The alkaline copper sulfate is added as Fehling
solutions A and B (A: copper sulfate. B: sodium hydroxide and sodium potassium tartrate). The unreacted
excessive Cu(II) is reduced by iodide and a correspoding amount of iodine is generated. This iodine is then
titrated with sodium thiosulfate (0.1 M Na2S2O3). Indication by platinum ring redox electrode.
Results
Sample Mean g/L RSD % n
White wine 0.983 0.53 4
Red wine 3.425 0.66 6
Orange juice 47.89 1.2 5
Grape juice 135.6 0.51 3
Fast and accurate moisture information is crucial for optimal control in sugar production plants and for the safe
storage and transportation of the final product of sugar refinement. Adjusting the moisture content to optimal
levels during the drying process and keeping it within tight tolerances, optimizes the production in order to
achieve the best quality.
The optimal moisture content of white sugar is typically between 0.01 and 0.05% and between 0.1 and 1.10%
in raw sugar.
It is also important to specifically know the water content. Since water contributes to the weight of sugar, it is
relevant to know its exact amount in order to obtain a meaningful product quality parameter. The surface water
content of granulated sugar is a critical parameter for its transformation into cubes as well as for silo storage.
5.1.5 Conclusion
The moisture content of sugar is determined fast and accurately with the easy-to-use Halogen Moisture
Analyzer. The results correspond fully with the reference method. Quick and precise moisture content results can
significantly contribute to the operational efficiency of sugar refineries and sugar processing companies.
In order to better accommodate for the rather low surface water content, external extraction with chloroform and
subsequent coulometric titration is the recommended alternative to the above described easy direct volumetric
procedure.
Apply the Compact Coulometric Karl Fischer Titrator C30.
5.2.2 Remarks
Methanol/formamide 1:1solvent was rather frequently used in the past to dissolve sugar completely. However, the
poisonous (teratogenic) formamide is mainly replaced by using the solvent for two-component reagent and a
homogenizer.
Also a jacketed titration vessel can be applied in order to carry out the analysis at elevated temperature, e.g. at
45 °C, to improve the dissolution of sugar samples. The dissolution of sugar is also faster at higher temperature.
Therefore, the minimum titration time can be reduced, e.g. to 600 seconds, which shortens the total analysis
time and increase the efficiency considerably.
5.2.3 Conclusions
For sugar, the Karl Fischer titration is a suitable method to determine either the total water content or the surface
water selectively. Appropriate solvents, procedures and methods are tested and available. The homogenizer
action is control-led by the titrator’s method. The titration control parameters are fine-tuned accordingly.
The major raw sugar refining techniques are the carbonatation and the phosphatation process. In both
processes a precipitate is formed which intraps and absorbs colorants and other impurities. Both processes
need careful control and monitoring to reach yield, efficiency and quality targets. Thus, quality controls of the
sugar production process in sugar refineries are fundamental.
The carbonatation is mainly applied to the sugar beet purification processing. Depending on region and
technical status quo, sugar cane processors apply the phosphatation or the carbonatation process.
6.4 Advantages
The system will run 24 hours a day during the harvest campaign and measures samples hourly. To be confident
that no process steps are out of limits during production, the range of results is defined within the method. If
any one sample is out of the defined limits, an alarm is generated and the operator can see this clearly on the
display. Immediate actions can be taken to optimize the production process without losing time and materials.
All methods and results are stored in the LabX® pro titration software and can be transferred to the LIMS System.
Figure 5: Fully automated titration system. METTLER TOLEDO Titration Excellence T90 with sample changer Rondo 20.
Several methods about sugar content determination have been presented in this paper. There are methods for
sugar content determination in liquids and solids with refractometers and density meters. Automated solutions
offer a higher accuracy and repeatability than manual instruments.
A quality aspect of sugar as a food ingredient is the moisture/ water content. Karl Fischer titration surely is the
most accurate solution to determine the water content. However, halogen moisture analyzers are a fast and
robust solution to quickly determine the moisture content of sugars on the production line.
METTLER TOLEDO supplies food laboratories with the right instruments, for the corresponding choice of method.
Find out more about our products, and get in touch with our experts, for suggestions on how you can benefit
from METTLER TOLEDO's expertise in the food industry.
If you liked this guide, we are proudly presenting the METTLER TOLEDO series of guides for the food industry.
Please click on the below links to get access to the respective food guides.
Application Brochures
Determinations in Beverages, Application Brochure Nr 19, Mettler Toledo 51725013
Good Density and Refractometry Practice™, read brochure on www.mt.com/gdrp
Karl Fischer Titration with a Homogenizer, Application Brochure Nr 27, Mettler Toledo 51725053
External sources
Wikipedia, e.g. http://de.wikipedia.org/wiki/Zucker
Wissenschaftszentrum Weihenstephan, e.g. http://www.wzw.tum.de/~bmeier/pages/83rebelein.htm
9. Appendix
Ti-Note Food & Beverage No. 10 Reducing Sugar Determination in Beverages According to Rebelein
Ti-Note Food & Beverage No. 16 Formol Number, Acidity and True Brix Value of Orange Juice
5
Routine 1
Operation Evaluation
Good
Measuring
4
Calibration / Practices 2
Qualification Selection
3
Installation /
Training
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