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Selected Analytical Methods: For The Sugar Industry
Selected Analytical Methods: For The Sugar Industry
Selected Analytical Methods: For The Sugar Industry
41
Application Brochure
Balances
pH Meters
Refractometers
Karl Fischer Titrators
Spectrophotometers UV/VIS
Halogen Moisture Analyzer
Excellence Line Titrators
Content 3
Introduction 4
Laboratory Solutions 5
Process Overview 5
ICUMSA Sugar Solution-Color Assessment 6
From Standalone to Fully Automated Systems 6
Fully automated measurement system 7
Common Procedure and Materials 8
Method GS1/3-7 9
Solution Colors at pH 7.0 of Raw and Specialty Sugars 9
Method GS2/3-9 10
White Sugar Solution Color at pH 7.0 10
Method GS2/3-10 11
White Sugar Solution Color 11
Method GS9/1/2/3-8 12
Solution Colour by the MOPS Method 12
Moisture Determination in Sugar 14
Process Optimization and Lab Efficiency 14
Halogen Moisture Analysis 15
Material and Methods 16
Correlation HX204 versus Drying Oven 17
Conductivity Ash Measurement 18
According to ICUMSA GS2/3-17 18
Conductivity Ash Measurement 20
According to ICUMSA GS1/3/4/7/8-13 20
Efficient Sugar Content Determination 22
Of Molasses and Syrups 22
Purification Process Monitoring by Titrimetric Analyses 24
®
One Click Water Determination 26
Of Raw Sugar 26
Amazing Weighing Solutions 27
For Different Applications 27
METTLER TOLEDO
Application Solutions Sugar
3
Introduction
Introduction
Sugar is important; all organisms need sugar as a source of energy. Its chemical structure
is simple, encompassing all saccharides from monosaccharides, disaccharides, oligo- and
polysaccharides. However, in everyday terms we think of sugar as a sweet crystalline
substance obtained from various plants. It is in fact sucrose, a disaccharide consisting of
fructose and glucose.
In earlier days, sugar was traded as a precious good, only affordable by the wealthy.
Today it is a commodity found in every grocery store. We find sugar in many foods,
beverages and even pharmaceutical products; but even though sugar is important for a
balanced metabolism, too much can have an adverse effect on our health.
Regardless of whether sugar is produced from sugar cane or sugar beet, it must meet the
standards defined by the industry and health organizations. By far the most important,
ICUMSA™ (International Commission for Uniform Methods of Sugar Analysis), is used as a
reference across the industry.
This includes:
• Color determination
• Brix values
• Moisture determination
• pH measurements
• Weighing solutions
• Karl Fischer water determination
• Titrimetric alkalinity and hardness analysis
4 METTLER TOLEDO
Application Solutions Sugar
Laboratory Solutions
For the Sugar Industry
METTLER TOLEDO offers a comprehensive range of analytical instruments and balances for efficient and reliable
quality control in the sugar industry. In the following we present a selection of instruments frequently used at
different process stages. All instruments are designed for easy operation, robustness and reliability. Sugar or
sucrose is produced from either sugar beet or sugar cane. The different production processes are shown below.
photom o-
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tomete
Titrato
Titrato
Balanc
Moistu
Balanc
Spectr
Analyz
Analy ti
Precis
pH m e
Karl Fis
Refrac
• • • • • •
• • • • • •
A, B1 & B2
METTLER TOLEDO
Application Solutions Sugar
5
ICUMSA™ Sugar Solution-Color Assessment
ICUMSA Color Determination
From Standalone to Fully Automated Systems
The color of sugar solutions, determined according to ICUMSA1, is one of the most important parameters refiners
assess [1]. METTLER TOLEDO offers safe and efficient ways to perform automated ICUMSA™ sugar-color assess-
ments, saving hours of manual transcription work.
Today, determining the final color value of sugar samples still requires many manual steps. Beginning with a
solution’s Brix value and reading its concentration from the ICUMSA table, through to measuring absorbance at
420 nm, all values are first recorded manually on paper before being transferred to a computer program for final
result calculation.
Not only are these steps time-consuming, they also bear the risk of transcription errors.
METTLER TOLEDO offers efficient and error-free analytical workflow systems to automatically calculate color
according to ICUMSA. From standalone to multi-instrument, all systems have in common to massively reduce
above mentioned manual data handling steps. Thus they can save up to several hours per week of operator
time, and help to minimize the risk of transcription errors. Further, the final color result can immediately be vali-
dated, as it is shown directly on the UV/VIS instrument’s screen.
Sample
Figure 1: By connecting a METTLER TOLEDO R4 and UV5 to the Figure 2: Standalone system using METTLER TOLEDO’s UV/VIS
LabX PC software, the ICUMSA color is automatically calculated Spectrophotometer to automatically calculate ICUMSA color.
and immediately shown on the instrument. The Brix value is entered manually in the field “correction factor”.
The LabX® software enables the connection and remote control of different instruments for multiparameter
measurements. In addition to storing data and meta-data, LabX automatically and securely transfers results
between instruments – in this case between the R4 and the UV5 – with users fully guided through the workflow.
By connecting a METTLER TOLEDO balance to LabX, this guidance can begin as early as weighing a sample.
All results, including from balances and pH meters, can be stored in LabX’s central database. A customizable
report is stored electronically; and where required, printed automatically. All data can also be transferred from
LabX to other laboratory information management systems (LIMS).
1
ICUMSA™ is a trademark of ICUMSA Ltd. and Verlag Dr. Albert Bartens KG.
6 METTLER TOLEDO
Application Solutions Sugar
Fully automated measurement system
For high-throughput demand METTLER TOLEDO offers automated sample handling options by connecting
an InMotion or SC30 autosampler to the R4 and UV5. After filtration, sugar solutions are transferred into
the respective lnMotion beakers or SC30 glass vials and placed on the Rack. From there the samples are
automatically processed, including automated barcode reading. Figure 3 shows the setup of such a fully
automated ICUMSA color-measurement system.
SD660
Waste
SPR200
Empty beaker
(blank UVVIS)
InMotion
Autosampler Samples
Water
R4
UV5
PowerShower
LabX
Figure 3: Fully automated ICUMSA color measurement system. After filtration, sugar solution samples are transferred into beakers and
placed on the InMotion. From there the samples are automatically transported to first measure the Brix on the R4 and then the absorbance
at 420 nm. All results are automatically shown on the instrument screen and securely saved in the LabX database.
METTLER TOLEDO
Application Solutions Sugar
7
ICUMSA Methods for Color Determination
ICUMSA Color Determination
Common Procedure and Materials
ICUMSA Method Titel • Use RDS to obtain the density of the test solution,
GS1/3-7 Solution Colours at pH 7.0 of Raw and ρ [7].
Specialty Sugars [2].
• Calculate the concentration of sample solids in
GS2/3-9 White Sugar Solution Colour at pH 7.0 [3].
solution from RDS [7].
GS2/3-10 White Sugar Solution Colour [4].
• Determine absorbance As at 420 nm using water
GS9/1/2/3-8 Sugar Solution Colour by the MOPS Method
as blank.
[5].
• Calculate the colour in ICUMSA units
8 METTLER TOLEDO
Application Solutions Sugar
Method GS1/3-7
Solution Colors at pH 7.0 of Raw and Specialty Sugars
Preparation of sample Table 2: Mean values (n=5) from measured raw sugar samples at
different concentrations and using different path lengths. The stan-
1. Prepare the solution by weighing defined sugar dard deviation (Std Dev) and the relative standard deviation (Srel)
and water aliquots according to the ICUMSA color were calculated. All color values are given in IU7.0.
ranges.
Sample White 1 White 2 Brown 1 Brown 2
Table 1: Aliquots of sugar, water and path length (b) Sugar solution (%) 30 50 30 10
Path length (cm) 5 2 1 1
ICUMSA color Sugar Water Path length Mean color (IU7.0) 280 340 600 4080
range aliquot (g) aliquot (g) (cm)
Measured 0 0 20 10
250-500 50 ± 0.1 50 ± 0.1 2* absolute
250-500 30 ± 0.1 70 ± 0.1 5* repeatability*
500-2000 30 ± 0.1 70 ± 0.1 1 Max. permitted NA NA 110 300
repeatability
2000-7000 10 ± 0.1 90 ± 0.1 1
Std Dev 0.0 0.0 5.5 4.5
7000-13000 5 ± 0.1 95 ± 0.1 1
Srel (%) 0.0 0.0 0.9 0.1
METTLER TOLEDO
Application Solutions Sugar
9
Method GS2/3-9
ICUMSA Color Determination
White Sugar Solution Color at pH 7.0
Preparation of sample
Table 1: Mean values (n=5) from two white sugar samples. The
1. Weigh 50 ± 0.1 g of sugar into a 250 mL flask. standard deviation (Std Dev) and the relative standard deviation
2. TEA/HCl buffer pH 7.0: Fill 500 mL of 0.1 mol/L TEA
into a 1000 mL beaker. Add 0.1 mol/L HCl until Sample White 1 White 2
the solution reaches a pH of 7.0 (approx. 420 mL). Sugar solution (%) 50 50
Store the buffer at 4 °C for up to one week. Path length (cm) 5 5
Adjust to room temperature before usage. Mean color (IU7.0) 86 362
3. Add 50 ± 0.1 g of TEA/HCl buffer. Dissolve the Std Dev 0.9 0.0
sample completely by stirring at room temperature. Srel (%) 1.0 0.0
4. Filter the solution under vacuum through
a 0.45 µm nc membrane filter in a clean flask. (Srel) were calculated. All color values are given in IU7.0.
5. Degas the solution in an ultrasonic bath The used automated result calculation yields in sig-
for 3 minutes. nificant time gains compared to manual transcriptions
and result calculations. Also, the risk of typing errors
Refractometer measurement parameters can be drastically reduced.
Taking into account the properties of the TEA/HCl
buffer, the RDS needs to be corrected by a factor All results, including from balances and pH meters,
0.989 (see Result 3). can be stored in LabX’s central database. A customiz-
Measuring able report is stored electronically; and where required,
temperature 20.00 °C printed automatically.
Result 1 T[Brix_ICUMSA_nD(nD)]/100
Result 2 The density (ρ) is calculated in LabX
according to the respective ICUMSA
formulas [4].
Result 3 The concentration (c) is calculated in
LabX as follows:
c = 0.989 RDS∙ρ∙10-5 g/mL.
Results
Table 1 summarizes results obtained from 2 different
white crystalline sugars.
10 METTLER TOLEDO
Application Solutions Sugar
Method GS2/3-10
White Sugar Solution Color
METTLER TOLEDO
Application Solutions Sugar
11
Method GS9/1/2/3-8
ICUMSA Color Determination
Solution Colour by the MOPS Method
Preparation of sample Table 1: Mean values (n=5) from different sugar samples. Standard
deviation (Std Dev) and relative standard deviation (Srel) were
1. Weigh sugar samples according to the following calculated.
table into a 250 mL conical flask.
Sample White 1 White 2 Brown 1 Raw 1
Pathlength cm ICUMSA Color Range Sugar Aliquot (g) Sugar solution (%) 20 20 10 5
Up to 800 20 ± 0.04 Path length (cm) 5 5 2 1
5 200-1,600 10 ± 0.02
400-3,200 5 ± 0.01 Mean color (IU7.0) 96 184 679 3072
12 METTLER TOLEDO
Application Solutions Sugar
Since the sugar production industry began in the 19th century, sugar has become
commonplace. It is consumed around the world every day in foods and drinks and
is used in other areas, such as in pharmaceutical products.
As sugar is used for so many purposes it needs to comply with many requirements.
Regardless whether sugar is produced from sugar cane or sugar beet, analyses
establish purity, content, processability and shelf-life.
METTLER TOLEDO
Application Solutions Sugar
13
Moisture Determination in Sugar
Moisture Determination
Process Optimization and Lab Efficiency
Keeping the moisture content of sugar and its co-products strictly within specifications is key
to the operational excellence of sugar plants.
This chapter describes how METTLER TOLEDO Excellence Moisture Analyzers speed up the
analysis of sugar and its co-products (pulp, pellets, bagasse) and deliver precise data on
moisture content within minutes. The fast results ensure accurate process control in
factories processing sugar beet and sugar cane.
HX204
Excellence Moisture Analyzer
14 METTLER TOLEDO
Application Solutions Sugar
Halogen Moisture Analysis
This article illustrates the fast moisture determina- Moisture in sugar – it’s the law, and key
tion of sugar and its co-products (pulp, pellets) in the to product quality
sugar factory using a METTLER TOLEDO Excellence Optimal moisture content of white sugar is typically
Moisture Analyzer. between 0.01 and 0.05%, and of raw sugar between
0.15 and 1.10%. International guidelines such as
Moisture analysis in sugar factories Codex Alimentarius 1, EU sugar policy 2 and national
Fast and accurate information on moisture content is guidelines (e.g. animal feed and fertilizer regulations)
crucial for optimal control of sugar production plants state quality requirements for sugar and sugar co-
and for the safe storage and transportation of the final products (pellets, bagasse, pulp). For example, refined
product. Typical points for measuring moisture in the or white sugar may have a maximum of 0.06% mois-
processing of sugar cane and sugar beet are illus- ture according to EU sugar policy. Adjusting the mois-
trated below. METTLER TOLEDO offers the full range ture content to optimal levels during the drying process
of analytical equipment required, including refractom- and keeping it within tight tolerances optimizes the
eters, balances, titrators and moisture analyzers. production for best quality.
1
Codex Alimentarius is a food standard developed by FAO and WHO
2
Commission Regulation (EC) No 1262/2001
3
Approx. 10,000 EUR per year in a German sugar refinery
METTLER TOLEDO
Application Solutions Sugar
15
Material and Methods
Moisture Determination
1. Select shortcut:
“White Sugar”
Method Settings:
Resolution: High (0.1 mg)
Preheating: 100 °C
Switch-off criterion: Free (1 mg/180 sec)
Drying Program: Standard
Drying Temperature: 105 °C
Start weight: 20 g
Same method parameters are applicable for
raw sugar.
Results
The moisture content of white sugar is mea- of both EU sugar policy regime 2 (maximum
sured with the HX204. The result obtained 0.06%, loss on drying) and the Codex
is 0.017 %MC. The result fulfills the criteria Alimentarius 1 (below 0.1%, loss on drying).
See Annex 1 for information on the oven drying reference method for sugar products
See Annex 2 for information on moisture analysis with the HX204 for sugar products
1, 2
Please see references on previous page.
16 METTLER TOLEDO
Application Solutions Sugar
Correlation HX204 versus Drying Oven
To prove the precision of the HX204 results, for sugar to be clarified with moisture respon-
a comparison study with sugars and sible. The study shows that the HX204
co-products was undertaken. Results from achieves highly repeatable results, fully cor-
the HX204 were compared to the drying oven responding to the drying oven method, with
method according to ICUMSA GS2/1/3/9-15 results in minutes instead of hours.
0.400 14.000
12.000
0.300
10.000
MC [%]
MC [%]
0.200
8.000
0.100 6.000
0.000 0.000
1 2 3 4 5 6 7 1 2 3 4 5 6
Measurement Measurement
HX204 - White Sugar Drying oven - White Sugar HR83 - Pellets Drying oven - Pellets
HX204 - Raw Sugar Drying oven - Raw Sugar HR83 - Dried Pulp Drying oven - Dried Pulp
Conclusion
The moisture content of sugar and sugar drying reference method. Fast and precise
co-products can be determined quickly information on moisture content can
and accurately with the easy-to-use HX204 significantly contribute to the operational
Excellence Moisture Analyzer, with results efficiency of sugar refineries and sugar
fully corresponding to the oven processing companies.
METTLER TOLEDO
Application Solutions Sugar
17
Conductivity Ash Measurement
Conductivity Ash
According to ICUMSA GS2/3-17
This method is used to determine the conductivity ash in white sugar and specialty sugar. This parameter gives
a measure of the concentration of inorganic impurities present in sugar. For this, 28 g of sample are dissolved in
deionized water to give a solution mass of 100 g, and then the conductivity of the solution is measured.
Waste disposal None • Pay attention that the measuring cell is completely covered
• Start measurement and follow the instructions on the display
Vijay Patil/ Puja Surve
Author, Version IMSG pH Lab • At the end of the measurement take the electrode out of the
Version 1.0 sample solution and rinse it with deionized water
Remarks
• The temperature of the deionized water and the sample must be
between 15 °C and 25 °C. If the temperature of sample/deionized
water exceeds this limit, measurement will stop automatically.
Formula
% (m/m) = 0.0006 x (
K1
1+0.026 x (T–20)
)– 0.35 x( 1+0.026K x (T–20))xK
2
Results
Parameter Results Temperature [°C] Limits
R3 [Sugar] 0.03% - -
R2 [Temperature of sample] 23.4 OK
R2 [Temperature of water] 23.2 OK
U1[2] 66.45 µS/cm 23.4 -
U1[1] 38.56 µS/cm 23.2 -
18 METTLER TOLEDO
Application Solutions Sugar
Comments
• In the case of liquid sample, the amount of sample taken must be such that the test solution contains 28 g
sample / 100 g of solution
• Conductivity ash cannot be directly compared with the gravimetric ash determined by incineration and
weighing of the ash
• The factors converting conductivity to conductivity ash are chosen in such a way that the conductivity ash
value corresponds approximately to values for sulfated ash. This is a conventional coefficient and cannot be
verified by experimental means.
Literature: ICUMSA Method GS2/3/9-17 The determination of conductivity ash in refined sugar products
and in plantation white sugar – Official (2011), Conductivity Guide (METTLER TOLEDO Analytical)
Method
Title Result limits yes
Method type Measurement Lower limit 15.0
Method ID M009 Upper limit 25.0
Conductivity ash measurement Interrupt outside limit yes
Title
acc. to ICUMSA GS2/3-17 Instruction
Author METTLER TOLEDO Place the sensor in the sugar
Instruction
Created on 2012-09-17 08:00:00 solution
Modified on 2012-09-17 08:00:00 Continue after Confirmation
Modified by METTLER TOLEDO Condition no
Protect yes Measure
SOP no Sensor name
Configuration Conductivity mode Conductivity
Measurement type Conductivity Unit µS/cm
Sensor name Decimal places 2
Temperature capture Internal Temperature correction Off
Temperature type 2 None Endpoint type Automatic
Sample Endpoint criteria standard
Sample ID SAMPLE01 Stir no
Comment - Condition no
Instruction Calculation
Place the sensor in the water Name Temperature range check
Instruction used for preparing the sugar Unit °C
preparation
Formula T1[2]
Continue after Confirmation
Decimal places 1
Condition no
Result limits Yes
Measure
Lower limit 15.0
Sensor name
Upper limit 25.0
Conductivity mode Conductivity
Interrupt outside limit yes
Unit µS/cm
Calculation
Decimal places 2
Name Sugar
Temperature correction Off
Uni %
Endpoint type Automatic
0.006*((U1[2]/
Endpoint criteria standard (1+0.026*(T1[2]-20))-
Formula
Stir no 0.35*(U1[1]/ (1+0.026*
Condition no (T1[1]-20))))
Unit °C Report
Decimal places 1
METTLER TOLEDO
Application Solutions Sugar
19
Conductivity Ash Measurement
Conductivity Ash
According to ICUMSA GS1/3/4/7/8-13
This method is used to determine the conductivity ash in raw sugar, brown sugar, juice, syrup and molasses. It
gives a measure of concentration of inorganic impurities present in the sugar solution. For this 5 g of sample is
dissolved in deionized water to give a solution mass of 100 g, and then the conductivity of the solution is mea-
sured. The results is reported in percentage.
Waste disposal None • Make sure that the measuring cell is completely covered
• Start measurement and follow the instructions on the display
Vijay Patil/Puja Surve
Author, Version IMSG pH Lab • At the end of the measurement take the electrode out of the sample
Version 1.0 solution and rinse it with deionzed water
Remarks
• The temperature of the solution must be between 15 °C and 25 °C. If
the temperature of sample/de-ionized water exceeds this limit, mea-
Formula surement will stop automatically.
% (m/v) = • In the event of the conductivity of sample exceeding 500 µS/cm, re-
0.0018 x ( ) – ( 1+0.023K x (T–20) )x K duce the solid content of the solution. (for molasses use
K1 2
1+0.023 x (T–20) 0.25 g/100 mL solution mass)
20 METTLER TOLEDO
Application Solutions Sugar
Results
Parameter Value Temperature [°C] Limits
R3 [Sugar] 0.11% - -
R2 [Temperature of sample] 23.4 °C - OK
R2 [Temperature of water] 22.7 °C - OK
U1[2] 114.07 µS/cm 23.4 -
U1[1] 45.47 µS/cm 22.7 -
Comments
• Conductivity ash cannot be directly compared with the gravimetric ash determined by incineration
and weighing of the ash
Literature: ICUMSA Method The determination of conductivity ash in raw sugar, brown sugar, juice,
syrup and molasses – Official (1994), Conductivity Guide (METTLER TOLEDO)
Method
Title Decimal places 1
Method type Measurement Result limits yes
Method ID M010 Lower limit 15.0
Conductivity ash measurement Upper limit 25.0
Title
acc. to ICUMSA GS1/3/4/7/8-13 Interrupt outside limit yes
Author METTLER TOLEDO Instruction
Created on 2012-09-17 08:00:00 Place the sensor in the
Instruction
Modified on 2012-09-17 08:00:00 sugar solution
Modified by METTLER TOLEDO Continue after Confirmation
Protect yes Condition no
SOP no Measure
Configuration Sensor name
Measurement type Conductivity Conductivity mode Conductivity
Sensor name Unit µS/cm
Temperature capture Internal Decimal places 2
Temperature type 2 None Temperature correction Off
Sample Endpoint type Automatic
Sample ID SAMPLE01 Endpoint criteria standard
Comment - Stir no
Instruction Condition no
Place the sensor in the water Calculation
Instruction used for preparing the sugar Name Temperature range check
preparation
Unit °C
Continue after Confirmation
Formula T1[2]
Condition no
Decimal places 1
Measure
Result limits Yes
Sensor name
Lower limit 15.0
Conductivity mode Conductivity
Upper limit 25.0
Unit µS/cm
Interrupt outside limit yes
Decimal places 2
Calculation
Temperature correction Off
Name Sugar
Endpoint type Automatic
Unit %
Endpoint criteria standard
0.0018*((U1[2]/
Stir no Formula (1+0.023*(T1[2]-20)) -U1[1]/
Condition no (1+0.023*(T1[1]-20))))
Calculation Decimal places 2
Name Temperature range check Result limits no
Unit °C Report
Formula T1[1] Print no
METTLER TOLEDO
Application Solutions Sugar
21
Efficient Sugar Content Determination
Sugar Content Determination
of Molasses and Syrups
The sucrose content of solutions containing mainly sucrose (e.g. molasses or syrups) is measured regularly for
quality control purposes. There are two main ICUMSA methods used: i) method GS4/3-13 (2007) which
describes the determination of the refractometric dry substance (RDS %) using an Abbe type refractometer and
ii) method GS4-15 (1994) describing the determination of apparent dry substance (°Brix) of molasses using a
hydrometer. METTLER TOLEDO’s bench top Refracto- and Density meters are suitable for both these methods.
22 METTLER TOLEDO
Application Solutions Sugar
Methods GS4/3-13 (2007) Sample Preparation
GS4-15 (1994) 1. Tare the beaker and weigh 50 g ( ± 0.5 g) of molasses. Re-
Instruments D4/D5 Density Meter cord the mass of molasses. Add 50 ± 1 mL of distilled water.
Automation unit (SC1 or SC30) Record the total mass of molasses and water. Mix the molasses
PPU drying pump and water thoroughly to ensure that a uniform solution of mo-
Balance (PB1502) lasses has been obtained.
Samples Molasses 2. Pour the solution into clean 20 mL sample vials, place them
into the automation unit and perform the measurement as de-
Method Temp. R.I. 20.00 °C scribed in the instrument manual.
Parameters Stability: 2 It is recommended to activate the repeat measurement function in
Wait time: 0 s order to prevent erroneous readings due to air bubbles or solid
Limit time: 300 s particles in the sample.
Sequence: On Results (n = 5)
Sampling Seq. : Auto Brix Refractive Index: 37.27% BrixnD, SD: < 0.01% BrixnD
Samp. Limit: 0 s Brix Density: 37.93% Brixd; SD: 0.01% Brixd
O.S. Rate: 130% me (mass of molasses + water) = 100.5
Drain Seq. : Auto md (mass of molasses) = 50.1
Samp. Limit: 0 s
Drain Seq. : Auto Calculations
Drain Rate: 100% BrixnD (Molasses) = (37.27 x me)/ md = 74.74% = RDS %
Rinse-1 Seq. : Set Brixd (Molasses) = (37.93 x me)/ md = 76.06% = apparent dry
Rinse-1 time: 15 s substance
Rinse-2 Seq. : Set Remarks
Rinse-2 Time: 25 s To exclude possible measurement errors due to non-homoge-
Purge seq. : Set neous samples (e.g. air bubbles), an automatic threefold repeated
Purge Time: 30 s measurement is carried out for each sample, moving the sample
Cell Test: Off by 25% between each measurement. If the standard deviation be-
Calib. : Air & water tween the three measurement exceeds a certain value, this means
Conclusion This proposed method clearly demonstrates that an air bubble or an impurity was found in the sample.
that fully automated molasses measure-
ments are possible. As the samples are
highly viscous and sometimes solid at room
temperature, dilution of the molasses is
recommended.
The proposed setup allows the easy integration of a UV/VIS Spectrophotometer for ICUMSA color measurements
as described on page 7 of this brochure. If required, either pH or conductivity measurements can also be in-
cluded into the measurement loop.
The suggested parameters can also be used for measurements of Brix using an R4/R5 (plus SC1/ SC30 and
flow-through cell) according to method GS4/3-13 (2007) or by using a D4 (plus SC1/ SC30) according to
method GS4-15 (1994).
Note:
i) Brix readings based on the refractive index and density differ slightly from each other due to other substances in the molasses.
These additional substances have a different effect on the refractive index than on the density.
ii) The sample amount was adapted from the original methods as METTLER TOLEDO’s digital density measurement principle
requires less sample than the hydrometer method.
METTLER TOLEDO
Application Solutions Sugar
23
Purification Process Monitoring by Titrimetric Analyses
Titrimetric analyses
The sugar beet purification processing technique is limit, the operator can see this immediately on the
known as carbonatation. Depending on region and display, and thus is able to optimize the production
technical status quo, sugar cane producers apply process without losing time and materials. All methods
different technologies for juice purifications, such as and results are stored in the LabX software and can be
the carbonatation process or phosphatation process. transferred to the LIMS system, if required.
Titrimetric analyses, such as alkalinity, total lime and
total hardness, offer important data to the purification
control procedure in both sugar cane and sugar beet
Analysis 1 Hardness Determination
production processes. METTLER TOLEDO’s Excellence
Instruments T9 Excellence titrator, InMotion sample changer,
line titrators add security, speed and efficiency to this DGi115-SC pH sensor, DX240-SC (calcium ion
process control during sugar production. selective) sensor with a DX200 reference and
barcode reader
Samples Power water
Press lime filtrate
Thin juice
Thick juice
Description The determination of the total hardness of water
is based on a complexometric titration of calcium
and magnesium with an aqueous solution of the
di-sodium salt of EDTA at pH 10.
Tips • Calcium ionic selective electrode sensor is the
best choice to determine total hardness for
samples which are very turbid, such as power
water, press lime filtrate and thin and thick
juices.
• Thin and thick juice samples vary strongly in
color depending on the beet root (e.g. from
light to dark brown). Therefore, the colorimetric
indication using a Phototrode® DP5 is not rec-
ommended for this application. The changing
color of the samples gives different color dark-
ness by the addition of Erio T as indicator,
Automated Titration System
which results in a decreasing signal.
The complete analytical sequence can be performed
Analysis 2 Alkalinity Determination
automatically. The refinery worker inserts the sample
Samples • Pre-liming
onto the InMotion rack and starts the analytical pro- • Main liming
cess with One Click® of the touch screen. Depending • 1st carbonatation
• 2nd carbonatation
on the sample, the system measures pH, alkalinity
Description The samples are titrated with HCl 0.3571 mol/L
and total hardness with the corresponding method. to an endpoint of pH 8.2
Analysis 3 Total Lime Determination
Advantages Samples Mud recirculates
The system will run 24 hours a day during the harvest Milk of lime
1st carbonatation
campaign and measures samples hourly. To be con-
Description With the addition of hydrochloride acid, the sam-
fident that no process steps are out of limits during ple is titrated to pH 1. The CaCO3 is then decom-
production, the range of results is defined within the posed to CaO and CO2. The remaining CaO is
method. If any of the samples is out of the defined titrated with sodium hydroxide to endpoint pH 5.1
24 METTLER TOLEDO
Application Solutions Sugar
Process Step Process description Analytic Limits
Extraction by diffusion
Raw juice with 12–18% of sugar
at 70 °C
Milk of lime:
Milk of lime is added (Ca(OH)2) for 11–16 g CaO / 100 mL
- Total lime
clarification of non-sugar compounds
Juice purification by
which will be flocculated as calcium salts,
pre-liming
e.g. oxalates, phophates, sulphates,
invert sugar).
Samples milk of lime and
pre-liming Pre-liming:
Ca(OH)2 + (C2O4)2–
2OH –
CaC O 2 4 +
- pH
pH 11.1–11.8
0.13–0.19 g CaO / 100 mL
- Alkalinity
0.5–1.0 g CaO / 100 mL
- Total lime
2nd carbonatation:
pH 8.5–9.7
Introducing of lime kiln gas (approx. - pH
0.012–0.022 g CaO / 100 mL
44% CO2) so that the juice becomes - Alkalinity
Second Carbonatation filterable and therefore reducing the
mud recirculate calcium content.
Thin juice:
Filtration Thin juice with 14–16% sugar 0.03–0.04 g CaO / 100 g DM*
- Total hardness
Thick juice:
Evaporation Thick juice with 60% sugar 0.03–0.04 g CaO / 100 g DM*
- Total hardness
Molasses
Centrifugation
Sugar crystals
METTLER TOLEDO
Application Solutions Sugar
25
One Click® Water Determination
Titrometric Water Determination
of Raw Sugar
Water content is an important sugar quality control parameter. Volumetric Karl Fischer titration enables
the specific and selective determination of either the total water content or only the surface water content of
sugar. Since water contributes to the weight of sugar, it is important 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. The volumetric Karl Fischer titrators of the compact V30S
and Excellence line T7 and T9 offer everything necessary for fast and accurate water determination in
One Click®.
26 METTLER TOLEDO
Application Solutions Sugar
Amazing Weighing Solutions
For Different Applications
METTLER TOLEDO
Application Solutions Sugar
27
Good Measuring Practices
Five Steps to Improved Measuring Results
5
Routine 1
Operation Evaluation
Good
Measuring
4
Calibration / Practices 2
Qualification Selection
3
Installation /
Training
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For more information