Instruction Manual Edible Oils and Fats - en
Instruction Manual Edible Oils and Fats - en
Instruction Manual Edible Oils and Fats - en
Tintometer® Group
Handbook of Methods
Analytical procedures for the measure-
ment of edible oils and fats
0.5 g to 1.0 g
= / ± 1 mg
5 ¼"
Title No. Page
How to use 4
Taking a Sample 5
Sample Preparation 6
Measurement Decisions 8
The Sample 13
Troubleshooting 14
Lovibond® RYBN Colour CM1 16
AOCS-Tintometer Colour CM2 22
Chlorophyll CM3 28
Red and Yellow Values to Indian Standard - Sesame Oil, Mustard CM4 34
Oil, Mahua Oil
Red and Yellow Values to Indian Standard - Castor, Ground Nut, CM5 40
Coconut Oil
Red and Yellow Values to Indian Standard - Castor, Ground Nut, CM6 46
Coconut Oil
Red and Yellow Values to Indian Standard - Cottonseed Oil CM7 52
Beta Carotene CM8 58
EN Handbook of Methods 3
How to use
4 EN Handbook of Methods
Taking a Sample
Taking a Sample
Follow standards such as ISO 5555:2001 Animal and vegetable fats and oils — Samp-
ling.
The key aspects of this standard include:
• Use of stainless-steel sampling containers as these are the most suitable
• Types of suitable sampling instrument:
- Weighted sample can
- Weighted cage for sample bottle
- Valve sampling cylinder (sinker sampler)
- Bottom sampler
- Sampling tubes and scoops
• The importance of clean or gloved hands
• Protection of the sample from contamination (rain or dust etc.)
• Heating of oils to facilitate sampling
• Homogenisation of the oil to be sampled
• The taking and preparation of inhomogeneous fats
It is most important to ensure that the sample has not been contaminated and is a
representative sample of the homogeneous bulk of oil concerned.
EN Handbook of Methods 5
Sample Preparation
Sample Preparation
This is one of the most important steps to ensuring accurate and repeatable measure-
ments not only in the single laboratory but also when comparing results across multiple
laboratories. Care taken here will reduce errors and provide better measurements.
Filtration
The sample should be clear and free of particles before it is measured.
Filtration of oil samples can be achieved through a process of heating (for samples that
are highly viscous at room temperature) and gravity or vacuum filtration.
Sealed
Strong Clamp Vacuum
Particle
filter Add
Vacuum
Universal
Vacuum
Lab Quality Hose
Borosilicate Connection
Glass
The choice of filter pore size should be based upon the sample oil. Some experimenta-
tion will be required to obtain the optimum pore size which provides sample clarity in a
suitable timeframe.
When placed into a cold measurement instrument, some samples may crystallise
quickly upon contact with the cooler surface of the sample cuvette.
To avoid this, warm the instrument (if applicable, see section on measuring equipment)
with the empty sample cuvette before use.
6 EN Handbook of Methods
Sample Preparation
Please note that some instruments provide heated sample chambers. These are not
intended for use in bringing the sample to a suitable temperature but to maintain tem-
perature while the measurement is taken.
Thermal currents:
A B C
Thermal currents After stirring
forming within the sample
a sample
The heater in the instrument is not intended to be used for heating samples up to tem-
perature as it will be quite slow. It is only intended to stop heat being taken away from
the sample during the measurement cycle.
EN Handbook of Methods 7
Measurement Decisions
Measurement Decisions
There are four key decisions that must be made prior to measuring colour in oil con-
sistently:
1) The choice of colour scale to be used in communicating the colour data.
2) Visual versus automatic measurement.
3) The path length across which the colour will be measured.
4) Possible dilution of the sample
Choice of Scale
Colour scales are designed to replicate the range of colours specific to an application-
type or sample colour-type. There are a number of scales which are used for measu-
ring edible oil colour. Your supplier or customer will be working to an existing scale and
it is important to try and maintain colour communication within a single scale.
8 EN Handbook of Methods
Measurement Decisions
if users of visual measurement systems employ neutral filters to dull a bright sample,
but omit to report this in their results.
A Neutral standard of a particular value is equivalent to a combination of Red, Yellow
and Blue standards, so if there is a match using all four colours, it can be simplified
by removing the smallest number from all the colours. For example, 1.5R, 7.8Y, 0.2B,
0.5N is equivalent to, and should only be reported as, 1.3R, 7.6Y, 0.3N.
Practical Aspects of Lovibond® RYBN Measured in Visual Systems
The Lovibond® RYBN colour scale is the preferred colour scale when measuring Lovi-
bond colour as it most closely correlates with the way in which visual instruments are
designed to be used.
There are two working practices which are sometimes used in visual systems, to simp-
lify the comparison of samples with glass colour standards.
Lovibond® RY
Uses only the Red and Yellow glass standards when comparing two samples (or samp-
le with a standard). This will often lead to lower values in the reported match due to the
brightness difference in visual measurement systems. A higher variation between users
will be seen, as a more subjective decision on the match at different brightness levels is
being made. An RY result may be correct, but often a complete result requires Neutral
values as well.
Lovibond® RY 10:1
In some sample oils, there is a useful relationship between Yellow and Red colour va-
lues (where Yellow is approximately ten times the Red value). The 10:1 ratio is often a
useful point to start from when making a colour match, then improved to a more precise
match using the full gamut of Red, Yellow, Blue and Neutral. The RY 10:1 ratio is a
step in the process of achieving a good RYBN match, but it is not a final result.
Chlorophyll
• AOCS Cc-13d-55, Chlorophyll Pigments in Refined and Bleached Oils
Whilst not a colour scale, the content of chlorophyll in a number of edible oils can be
determined by light absorbance. The relationship between absorbance (optical density)
at 670nm, 630nm and 710nm is dependent upon the chlorophyll content of the oil.
The sample pathlength is used in the calculation of chlorophyll content and should be
EN Handbook of Methods 9
Measurement Decisions
chosen such that the optical density at 670nm is between 0.3 and 0.8.
Beta Carotene
• BS 684 (section 2.20) Determination of carotene in vegetable oils
Beta Carotene is seen in some oils (e.g. Palm Oil) as the orange/red hue. This can be
measured as light absorbance at 445nm. It should be noted that as a purely quantita-
tive method, any sample that absorbs light at 445nm will give a result (which may not
necessarily be constituted of beta carotene).
Automatic Measurement
• Consistent repeatability of results between instruments of the same principle and
design.
• Only requires a single operative to provide a result.
10 EN Handbook of Methods
Measurement Decisions
Because of the logarithmic nature of the Lovibond® RYBN colour space, when measur-
ing in Lovibond® RYBN, it is recommended to select a cell with a pathlength such that
the total of colour units required to match is not greater than 20 (R + Y + B or N <20).
Doing so will improve repeatability and reproducibility.
Linear Scale
0 10 20 30 40 50 60 70
Logarithmic Scale
0 10 20 30 40 70
Sample dilution
Sample Dilution for Lovibond® RYBN, Lovibond® RY, Lovibond® RY 10:1 or
AOCS Tintometer
Sample dilution is not recommended. Selection of a suitable pathlength will ensure
repeatable and reproducible results.
Sample Dilution for Beta Carotene
Dilute your sample in analytical grade cyclohexane at a dilution of 1:100. The PFXi and
Model Fx firmware assumes that the dilution is correct, so one must weigh out precise-
ly 1 g of oil, measured as accurately as possible (BS684 2:20 states one should use
scales accurate to 1mg) and dilute to 100 ml with cyclohexane.
Then measure in a 10mm pathlength cuvette.
One can avoid solvent dilution by using an undiluted sample and measuring in a
0.1 mm pathlength cuvette (part number 606700) with the measurement instrument
pathlength set at 10 mm.
10 mm Cuvette
EN Handbook of Methods 11
Measurement Decisions
Equipment Verification
As with any measurement device it is important that the instrument used for colour
measurement is checked to ensure that it is working within its specified parameters.
With colour measurement instruments this done by measuring standards with known
values against which the results can be compared.
12 EN Handbook of Methods
The Sample
The Sample
All vegetable oils contain the same fatty acids, oleic acid, linoleic acid, palmitic acid
and stearic acid. However, other fatty acids can also occur in sometimes significant
amounts and the matrix in which these fatty acids are contained are very different. This
leads to large practical differences in the physical and optical properties of these oils.
Sample Types
Lovibond® products are designed to measure all types of edible oils. The most common
oils covered in these methods are listed here:
• Soya bean oil
• Palm oil
• Rapeseed/Canola oil
• Sunflower seed oil
• Groundnut (peanut) oil
• Cottonseed oil
• Coconut oil
• Palm kernel oil
• Olive oil
• Corn oil
• Sesame oil
• Linseed oil
The viscosity, density and optical properties of these vary between each oil and with
temperature. This variance, along with the oil´s common visible spectral characteristics
influences both the way it is prepared for measurement and the colour scale to which it
may be measured.
EN Handbook of Methods 13
Troubleshooting
Troubleshooting
Common Issue Solution
Our Automatic Instrument (Lovibond Your samples are not transparent,
Model Fx or PFXi) is showing higher they require filtering or heating.
Blue values when compared to our
Visual Tintometer Model F.
Our samples are heated and transpa- Convection currents in your samples
rent, but we are experiencing differen- could be causing issues. Please stir
ces between our Automatic Instrument them before measuring.
(Lovibond Model Fx or PFXi) and
Visual Tintometer Model F.
Despite transparency, appropriate cell Your instruments and cells should be
path length and stirring we are still clear and in a good state of repair.
experiencing differences between our Oil contamination and damage can
Automatic Instrument (Lovibond Model negatively impact results.
Fx or PFXi) and Visual Model F.
Where can I get my instrument ser- Please contact The Tintometer Ltd for
viced? advice. We are happy to help.
Despite transparency, appropriate cell Review the relevant standard (e.g.
path length, stirring and cleanliness AOCS 13e-92) for recommended
we are still experiencing differences tolerances. Visual instruments are less
between our Automatic Instrument (Lo- repeatable than automatic.
vibond Model Fx or PFXi) and Visual
Model F.
We are getting different results from Check you are using the same colour
another site. scale, cell path length, temperature
and sample preparation technique.
Our Automatic Instrument (Lovibond Are you correctly compensating for
Model Fx or PFXi) is showing Neutral brightness when using your Tintome-
values when compared to our Visual ter Model F?
Tintometer Model F.
Our Automatic Instrument (Lovibond Check you are applying the correct
Model Fx or PFXi) is reporting Blue colour scale. Lovibond RYBN reports
and Neutral Values that we do not re- Red, Yellow, Neutral and Blue values.
port on our Visual Tintometer Model F. AOCS Tintometer reports Red and
Yellow only.
How can I check inter-instrument We recommend checking with a Lovi-
agreement between a Lovibond Model bond Universal Verification Standard
Fx, PFXi and/or Tintometer Model F. set.
When using our Visual Tintometer We strongly advise against this poor
Model F instrument we wish to round practice.
down Y values to the nearest 10.
14 EN Handbook of Methods
Troubleshooting
EN Handbook of Methods 15
Lovibond® RYBN Colour / CM1
Application List
• Food and Beverage
• Household Products
• Petroleum Oils and Waxes
• Edible Oils and Fats
• Chemicals
Applicable Standard
• AOCS Cc 13j-97
• ISO 27608
• MS 252 : Part 16
• MS 817 : Part 12
• AOCS Cc 13e-92
• BS684
• ISO 15305
Glass Standards
Title Packaging Unit Part Number
Lovibond Red, Yellow, Neutral Filter Set 1 pc. 185000
(Model F, E, D)
Lovibond Red, Yellow, Blue (Model F, E, D) 1 pc. 186000
Lovibond Red, Yellow, Neutral (Model F, E, 1 pc. 184000
D)
Lovibond Red, Yellow, Neutral Filter Set 1 pc. 139590
(PFXi 995/950/880)
Lovibond Red, Yellow, Neutral Filter Set 1 pc. 139610
(PFXi 995/950/880)
Lovibond Red, Yellow, Blue Filter Set (PFXi 1 pc. 139620
995/950/880)
Lovibond Red, Yellow, Neutral (PFXi 1 pc. 139630
995/950/880)
Lovibond Red, Yellow, Neutral (Fx) 1 pc. 169630
Lovibond Red, Yellow, Neutral Filter Set (Fx) 1 pc. 169610
Lovibond Red, Yellow, Blue Filter Set (Fx) 1 pc. 169620
Lovibond Red, Yellow, Neutral Filter Set (Fx) 1 pc. 169590
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Sample Preparation
100 ml
Stir sample to disturb Fill prepared sample in the Place cuvette containing
convection currents. sample cuvette to 75 % of Sample in the sample
maximum. chamber. Pay attention to
the positioning.
133.4 MM / 5 ¼“
76.2 MM / 3“
25.4 MM / 1“
12.7 MM / ½“
6.4 MM / ¼“
3.2 MM / ⅛“
Total ≤ 20
1.6 MM / 1/16“
Taking Measurement
Performing a Test: Model Fx, PFXi
Red =
Yellow =
READ Blue =
Neutral =
Temperature =
Pathlength =
Taking Measurement
Performing a Test: Model F
R = 8.4
R = X = 8.5
R = 8.6
Troubleshooting
Common Issue Solution
We are measuring Lovibond RYBN Shorten the cell path length used for
values of R+Y+B or N >20. more precise results.
We wish to measure Lovibond RYBN, but Select Lovibond RY on your Lovibond
only report (R)Red and (Y)Yellow. Model Fx.
We wish to measure Lovibond RYBN, but Select Lovibond 1:10 on your Lovibond
wish to fix the ratio at 1:10. Model Fx.
Application List
• Food and Beverage
• Household Products
• Edible Oils and Fats
Applicable Standard
• AOCS Cc 13b-45
• AOCS Cc 8d-55
• AOCS Cc 13j-97
Glass Standards
Title Packaging Unit Part Number
AOCS-Tintometer Filter Set (Fx) 1 pc. 166900
AOCS-Tintometer Filter Set (PFXi 1 pc. 136900
995/950/880)
AOCS-Tintometer Colour (AF 710-3) 1 pc. 109720
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Sample Preparation
100 ml
5 ¼“
133.4 MM / 5 ¼“
25.4 MM / 1“
R < 20
Y < /70
Taking Measurement
Performing a Test: AF710-3
R = 8.4 Red =
Y = 16.0
Yellow =
R = X = 8.5
Y = X = 15.8 Temperature =
R = 8.6 Pathlength =
Y = 15.6
Taking Measurement
Performing a Test: Model Fx, PFXi
Red =
READ Yellow =
Temperature =
Pathlength =
Chlorophyll CM3
Application List
• Food and Beverage
• Edible Oils and Fats
Applicable Standard
• AOCS Cc 13d-55
Glass Standards
Title Packaging Unit Part Number
Chlorophyll A (PFXi 995/950/880) 1 pc. 139530
Chlorophyll A (Fx) 1 pc. 169530
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Sample Preparation
100 ml
133.4 MM / 5 ¼“
READ 10 MM / 0.4“
1 MM / 0.04“
Place cuvette containing Press the READ button The method suggests
Sample in the sample (Model Fx: √ button) to take adjusting the cell path
chamber. Pay attention to measurement. length to ensure that
the positioning. the absorbances at 630,
670 and 710 nm all fall
between 0.3 and 0.8 A. As
a rough guide, 0 – 10 ppm
can be measured at 1”
to 5 ¼”, 10 – 20 ppm at
10 mm and >20 ppm at
1 mm.
Instrument Settings
Taking Measurement
Performing a Test: Model Fx, PFXi
READ
Chlorophyll =
Temperature =
Pathlength =
Application List
• Food and Beverage
• Household Products
• Petroleum Oils and Waxes
• Edible Oils and Fats
• Chemicals
Applicable Standard
• IS 548 (part 1)-2010
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Sample Preparation
50 ml
6.4 MM / ¼“
Clean Cell
CCl4 +
Clean the cuvette. Fill prepared sample in the Place cuvette containing
sample cuvette to 75 % of Sample in the sample
maximum. chamber. Pay attention to
the positioning.
Taking Measurement
Performing a Test: Model Fx, PFXi
Red =
Yellow =
READ Blue =
Neutral =
Temperature =
Pathlength =
Taking Measurement
Performing a Test: Model F
∑ Y + 5 ∑R =
Application List
• Food and Beverage
• Household Products
• Petroleum Oils and Waxes
• Edible Oils and Fats
• Chemicals
Applicable Standard
• IS 548 (part 1)-2010
Sample Preparation
50 ml
25.4 MM / 1“
Clean Cell
CCl4 +
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Taking Measurement
Performing a Test: Model Fx, PFXi
READ Y+5R=
Place cuvette containing Press the READ button Multiply the total Red
Sample in the sample (Model Fx: √ button) to take values by five and add to
chamber. Pay attention to measurement. total Yellow values to give
the positioning. result.
Taking Measurement
Performing a Test: Model F
∑ Y + 5 ∑R =
Application List
• Food and Beverage
• Household Products
• Petroleum Oils and Waxes
• Edible Oils and Fats
• Chemicals
Applicable Standard
• IS 548 (part 1)-2010
Sample Preparation
50 ml
6.4 MM / ¼“
Clean Cell
CCl4 +
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Taking Measurement
Performing a Test: Model Fx, PFXi
READ
Fill prepared sample in the Place cuvette containing Press the READ button
sample cuvette to 75 % of Sample in the sample (Model Fx: √ button) to take
maximum. chamber. Pay attention to measurement.
the positioning.
Y+5R=
Application List
• Food and Beverage
• Household Products
• Petroleum Oils and Waxes
• Edible Oils and Fats
• Chemicals
Applicable Standard
• IS 548 (part 1)-2010
Sample Preparation
50 ml
6.4 MM / ¼“
Clean Cell
CCl4 +
For this colour scale, a baseline measurement must be carried out in the following
devices: Model Fx, PFXi
ZERO
Ensure the measurement Press the ZERO button
chamber is empty and (Model Fx: Ø button) to
close the lid. perform a baseline.
Taking Measurement
Performing a Test: Model Fx, PFXi
READ Y + 10 R =
Taking Measurement
Performing a Test: Model F
∑ Y + 10 ∑R =
Application List
• Food and Beverage
• Edible Oils and Fats
Applicable Standard
• BS684 Section 2.20
Glass Standards
Title Packaging Unit Part Number
Beta carotene (PFXi 995/950/880) 1 pc. 139520
Beta carotene (Fx) 1 pc. 169520
Sample Preparation
50 ml
ZERO
10 mm
Fill 10 mm cuvette with Place sample vial in the Press the ZERO button
Cyclohexane sample chamber. • Pay (Model Fx: Ø button) to
attention to the positioning. perform a baseline.
Taking Measurement
READ
10 mm
Fill cuvette with prepared Place sample vial in the Press the READ button
sample in solution with sample chamber. • Pay (Model Fx: √ button) to take
cyclohexane. Please note attention to the positioning. measurement.
it is important for the oil
content to be as close to
1g in 100 ml as possible for
the best accuracy.
Beta Carotene =
Temperature =
Pathlength =
Record results.