Professional Documents
Culture Documents
bcr information
REFERENCE MATERIALS
The certification of
a tomato paste colour
reference tile
CRM 400
Commission of the European Communities
Community Bureau of Reference
bcr information
REFERENCE MATERIALS
The certification of
a tomato paste colour
reference tile
CRM 400
M. Kent
Torry Research Station
Aberdeen, UK
F. Malkin
Ceram Research Ltd
Stoke-on-Trent, UK
J.F. Verrill
National Physical Laboratory
Teddington, UK
D.J. Henshall
Campden Food Research Association
Chipping Campden, UK
LEGAL NOTICE
Neither the Commission of the European Communities nor any person acting on
behalf of the Commission is responsible for the use which might be made of the
following information
DISCLAIMER
Whenever, in this report, a commercial product is identified by the
manufacturer's name or label, such identification should in no instance
be taken as an endorsement by the Commission or as an indication that
the particular product or equipment is necessarily the best available
for the particular purpose
Printed in Belgium
Page
CONTENTS
1 Introduction
1.1 Background 1
1.2 Determination of tomato paste colour 2
1.3 Specification of the tiles 3
2 Participants
3 Preparation of Tiles
4.1 Methods 9
4.2 Results 10
5 Stability
6.1 Strategy 16
6.2 Preliminary calibration of the master tomato tiles 16
6.3 Results for master tomato reference tile (GM89) 17
6.4 Uncertainties in the calibration of the master tomato reference tile 25
6.5 Certified individual reference values and their uncertainties 26
6.6 Colorimeters calibrated in other scales 27
7 Instructions for Use
A.l Introduction 31
A.2 Scope and field of application 31
A.3 Materials 31
A.4 Apparatus 31
A. 5 Sampling and samples 32
A.6 Procedure 32
— III —
Annex B Intercomparison of Laboratories and Instruments
B.l Participants 35
B.2 Design of experiment 36
B.3 Results 37
References 41
— IV —
1 INTRODUCTION
1.1 Background
and justified some research effort. The Community production of tomato paste
Two important proposals of interest to the tomato industry arose out of this
work. They concerned (a) the need for standardisation of the method of colour
colour close to that of a good quality tomato paste product. In the first of
tile, proposal (b) above. Such a tile would not be for use as a target colour
for tomato paste but for the essential calibration of instruments. Obviously
the closer it is in colour to the product it represents then the more useful
it will be as a calibrant.
The Commission undertook, to produce and certify such a reference tile which is
quality criterion. This criterion is adopted for two major reasons, (1) the
flavour, and (2) the colour of tomato paste is of obvious importance for food
The need to have a common procedure for measurement of colour has been
recognised at both national and company levels and several schemes have been
However, these widely used scoring systems are based on measurements carried
out on fairly dilute pastes (8.5 X total soluble solids (TSS)) and as was
found in the C0ST90bis work, the problems associated with translucency and
colour measurement are more severe at such dilutions than say at 12 X TSS, ,a
instruments therefore have colour values which are somewhat removed from those
This report describes the preparation of ceramic reference tiles suitable for
work and after consultation with industrial users of tomato paste. These
total soluble solids content (TSS) and were, in Hunter L,a,b units^ '
It is stressed that these values were chosen exclusively for the purpose of
specifying the target values for the reference tile and do not in anyway
3-
2 PARTICIPANTS
4-
3 PREPARATION OF THE TILES
The Tomato Paste Reference Tiles were produced in the laboratories of Ceram
Research using the techniques developed for the production of the Colour
Standards which are certified and sold by the National Physical Laboratory
(NPL) <6><7>.
produced red pigments were strong enough for the task, it was necessary to
rely on batches of red pigment specially produced in the laboratory for the
red pigment batches with either black, or reddish-brown pigments. However, the
recipe including the brown pigment gave a closer match to the spectral curve
of tomato paste. At this point two prototype tiles were produced from this
The unglazed tiles used for the reference tiles were 101 x 101 x 8 mm nominal
size. They were rigorously selected for the purpose and checked to ensure
that the finished glaze tiles would have a slight convex curvature, and so
The bulk glaze was prepared and adjusted to give a satisfactory colour
-5
The glaze was applied to the 'biscuit' tiles using a laboratory waterfall
dipping line. Two coatings of glaze were applied, with the tile turned
Sufficient glaze was applied to give a fired glaze thickness of 0.30 mm.
The tiles were fired to 1060 °C with a 4 hour soak in an electric intermittent
kiln fitted with a microprocessor control system. As the kiln only holds some
600 tiles it was necessary to carry out three dipping and firing cycles to
produce sufficient glazed tiles. To check how well the firings repeated, a
sample of 30-40 tiles was taken from each firing and measured on the Hunterlab
Colorimeter. The mean colour values for each firing agreed very closely,
within ± 0.05 unit for L and b, and ±0.1 unit for a. All the tiles could
therefore be merged into one batch. In all some 1700 tiles were produced.
As the tiles were taken from the kiln they were given an initial visual
tiles was made in the laboratory in better lighting conditions. This resulted
after production before using them as colour standards. To check the Tomato
weekly intervals from the 4th week after production to the 10th week. The
standard deviations of the overall means of the results for the batch
designated as batch 'A' were for L, +0.02, for a, +0.04 and for b, +0.02.
Laboratory temperature fluctuated between 23.0 °C and 24.7 °C during the
measurements.
Part way through these tests the tiles in batch B were irradiated under
(This is in line with experience gained in the production of the red tile in
using a digital thermometer with a ribbon surface probe. The tile was placed
on the colorimeter and a reading was taken immediately. Readings were then
taken over a 15 minute period when the tile was removed and the surface
-7-
Table 1 Thermochromic changes in L,a,b values
Temp change/°C AL Aa Ab AE
Actual change +4.3 -0.18 -0.23 -0.13 0.32
The changes expected for a 1 °C temperature rise quoted above are calculated
on the basis of the well established fact that thermochromic changes are
Each tile has been sealed into a protective plastic backing tray to guard
against any risk of contamination of the porous tile body which might affect
its calibration. These backing trays carry the inscription 'BCR Reference
Tile'.
For permanent identification the number of the tile has been inscribed on one
corner of the front of the tile. The label fixed to the back of the tile
carries the number of the tile and its individual Hunter L, a and b values.
The Tomato Paste Reference Tiles are supplied in a fitted storage case.
8-
HOMOGENEITY OF THE BATCH
4.1 Methods
The instrument used to study the homogeneity of the batch was a Hunterlab
of the sample was by twin opposed beams incident at 45° while the detectors
were mounted normal to the sample. The Colorimeter was linked to a micro-
computer for data handling. All measurements were made in the Hunter L,a,b
system^5* at 25 °C.
subsequently with them rotated through 90°, 180°, 270° and 360° in the
Table 2 also. To obtain the total uncertainty at the 95% confidence level the
L a b a/b
Instrumental Repeatability 0.005 0.012 0.006 0.001
Day-to-Day Repeatability 0.04 0.06 0.03 0.003
Orientation Repeatability 0.04 0.12 0.03 0.012
Overall 0.056 0.135 0.043 0.012
The individual measurements on c. 1400 tiles could not be carried out in one
session. Therefore one tile was measured and used as a reference in all other
measurement all the tiles were cleaned and numbered. The calibration of the
4.2 Results
decided to remove the tiles with a-values below 32.25 (146 tiles) and those
with a-values above 33.25 (21 tiles) from the batch. This left a final batch
The mean and range of L,a,b values for these 1232 tiles are given in Table 3
together with original target values for comparison. Values are illustrated
tolerance from the target value, and the mean a,b and a/b-values are very
10
16
15
14
Hon
13
12
11 J I I I
29 30 31 32 33 34 35
a
11
27
26 P.
/
Production
mean
25 —
T.
/
24 Target colour
23 — ^ T o l e r a nee
22 1 1 1 1 f
29 30 31 32 33 34 35
a
12
Table 3 Tomato Paste Reference Tiles - Mean and range of L,a,b values
accepted for the final batch and compared with target range
L a b a/b
Targe t max 26.5 34.0 16.0 2.34
Target min 22.5 30.0 12.0 2.24
Batch mean 26.05 32.80 14.44 2.27
Production max 26.42 33.25 14.63 2.30
Production min 25.41 32.25 14.22 2.23
-13
5 STABILITY
Fifteen tiles have been taken, divided into 3 groups and stored in the
following conditions:
Measurements are being made on all 15 tiles at monthly intervals over a period
referred to the 1931 2° standard observerv '. In order to take account of any
instrument fluctuation due to lamp fading or any other cause, the colour
whose stability has been verified over some years. From Table A it can be
seen that those tiles stored in the dark at 2°C and 27°C suffered no
significant changes in L,a,b values over the period of 394 days; significant
that is both with respect to the quoted uncertainties in the certified Hunter
L,a,b values and with respect to the instrument repeatability (Table 12,
Section 6.5). The large excursions from the means at 231 days were probably
period of 394 days shows comparable values for both sets of tiles stored in
the dark and for the pink enamel standard. The fluctuations that occurred
reference colour. The tiles stored under illumination however show a marked
-14
decrease in L, a and b values reflected in the larger standard deviation of
the mean measurements. Changes of -0.2, -0.4 and -0.1 were observed in L, a
and b respectively over the first 2 weeks of storage for those tiles in bright
Table 4 Mean L,a,b values for th« 5 tiles in each batch compared with those for a reference pink enamel
til* (Standard No C2-13669, Hunter Associates Lab Inc., Fairfax, Virginia)
Reference Pink
Enamel Tile Illuminated at 27°C Dark at 27°C Dark at 2°C
Days
0 68.96 23.92 12.16 26.04 32.97 14.51 26.06 32.98 14.51 25.85 12.73 1L 4 . 4 5
6 68.94 23.89 12.19 25.83 32.55 14.29 26.00 32.91 14.43 25.83 12.70 1L4.41
27 68.96 23.85 12.20 25.88 32.50 14.29 26.02 32.88 14.44 25.86 12.65 ]L4.41
50 68.85 23.73 12.26 25.75 32.33 14.32 2S.99 32.75 14.47 25.95 12.65 :L4.52
70 68.92 23.68 12.28 25.82 32.28 14.34 26.08 32.77 14.53 26.02 12.59 ]L4.55
98 68.79 24.02 12.06 25.59 32.44 14.16 25.82 33.01 14.39 25.76 12.88 3L4.40
125 68.90 23.99-- 12.07 25.63 32.40 14.18 25.88 32.99 14.41 25.87 12.91 ]L4.47
147 68.87 23.92 12.13 25.65 32.38 14.22 25.90 32.94 14.43 25.88 12.84 1L4.48
184 68.96 23.85 12.17 25.69 32.29 14.21 25.96 32.89 14 . 4 6 25.95 12.80 ]1 4 . 5 0
231 68.83 24.07 12.02 25.50 32.32 14.08 25.69 32.92 14.31 25.81 12.94 11 4 . 4 3
288 68.96 23.78 12.22 25.64 31.97 14.08 25.84 32.64 14.33 25.88 12.64 IL4.42
336 68.83 23.88 12.10 25.63 31.92 14.07 25.84 32.71 14.40 25.79 12.59 JL4.42
363 68.93 23.87 12.12 25.67 31.87 14.07 25.88 32.69 14.40 25.85 12.58 1L4.44
394 68.90 23.77 12.13 25.77 31.71 14.06 25.94 32.66 14.45 25.87 12.53 IL4.<«
Mean 68.90 23.87 12.15 25.72 32.28 14.21 25.92 32.84 14.43 25.87 12.72 1 4.4:
s.d. +0.06 +0.11 +0.08 ±0.14 ±0.3 2 + 0.13 +0.11 ±0.13 +0.06 ±0.07 >t 0 . 1 4 ito.o;
15
6 CERTIFICATION OF THE INDIVIDUAL TILES
6.1 Strategy
The certification of L,a,b values of each tile depends upon the use of a
One of the tiles close to the mean colour has been designated Tomato Master
Tile (Ceram Research number 126: NPL number GM89) and has been calibrated by
intervals over the spectral range 380 nm to 780 nm. The half height bandwidth
varies continuously during the scan falling from a value of 0.5 nm at 780 nm
in the centre of the tile was used. Measurements were made in the normal/
diffuse (0/d: specular excluded), 8°/total (8/t: specular included) and 0°/45°
geometries. The reference was an MS 20 opal glass which had been calibrated
sequence reference scan, sample scan, reference scan. The dark reading was
subtracted from each reading. The reflectance relative to the reference was
16-
The spectral curve for this Master Tile and for the 0°/45° geometry is shown
plotted in Figure 4 where it is compared with the curves for a tomato paste
sample and an enamel standard which is currently used for tomato paste colour
measurement.
Note: for security, one other tomato tile has also been likewise calibrated
and 10 in the CIE x, y, Y system together with u' v' and CIELAB values.
- 17
60
BCR M a s t e r T i l e
* 40
u
O
*♦■ 30
<D
U
c
D
D 20
10
0
400 500 600 700
Wavelength (nm)
Figure 3 Spec
t ral curves measured using the 0°/45° geometry, for BCR
Master tile, a tomato paste sample and an enamel red tile
currently used as a tomato reference colour.
18
Table 5
Spectral Reflectance Factors (%) for 0/d geometry for
Tomato Reference Tile GM89 (Ceram Research No 126)
575 3.51
580 4.15
585 5.26
590 7.03
595 9.64
19
Table 6
Colorimetric Data
Geometry 0/d
Tomato Paste Reference Tile GM89 (Ceram Research No 126)
2 Degree Observer
Illuminant D65 0.5790 0.3447 6.44 0.3874 0.5189 30.5 41.9 33.0
10 Degree Observer
X y Y(%) u' V L* a* b*
Illuminant A 0.6365 0.3454 8.96 0.4336 0.5294 35.9 41.1 42.1
Illuminant D65 0.5719 0.3499 6.13 0.3778 0.5201 29.7 39.3 32.1
20-
Table 7
Spectral Reflectance Factors (%) for 8/t geometry
for Tomato Reference Tile GM89
575 9.54
580 10.20
585 11.32
590 13.13
595 15.78
21 -
Table 8
Colorimetric Data
Geometry 8/t
Tomato Paste Reference Tile GM89 (Ceram Research No 126)
2 Degree Observer
X y Y(%) u' V L* a* b*
Illuminant D65 0.4452 0.3355 12.52 0.2902 0.4921 42.0 29.4 15.7
10 Degree Observer
Illuminant D65 0.4383 0.3388 12.22 0.2833 0.4927 41.6 27.1 14.9
22
Table 9
Spectral Reflectance Factors* (%) for 0°/45° geometry for
Tomato Reference Tile GM89
575 3.47
380 0.51 580 4.13
385 0.53 585 5.26
390 0.56 590 7.05
395 0.60 595 9.72
775 56.33
780 56.66
*NB Also known as spectral radiance factors for this geometry for mainlj
historical reasons
23
Table 10
Colorimetric Data
Geometry 0°/45°
Tomato Paste Reference Tile GM89 (Ceram Research No 126)
2 Degree Observer
X y Y(X) u' v' L* a* b*
Illuminant A 0.6460 0.3378 9.25 0.4485 0.5277 36.5 45.9 44.1
Illuminant C 0.5861 0.3419 6.57 0.3953 0.5189 30.8 41.3 35.3
Illuminant D65 0.5862 0.3455 6.48 0.3925 0.5205 30.6 42.8 34.8
10 Degree Observer
X y Y(%) u' v' L* a* b*
Illuminant A 0.6394 0.3446 9.08 0.4367 0.5296 36.1 41.8 44.1
Illuminant C 0.5788 0.3474 6.23 0.3851 0.5201 30.0 38.9 34.3
Illuminant D65 0.5794 0.3508 6.16 0.3830 0.5218 29.8 40.1 34.0
-24
6.4 Uncertainties in the Calibration of the Master Tomato Reference Tile
The uncertainties in the spectral values for the 0/d and 8/t geometries are
dR
AR = ±(0.05 + 0.004R + 0.2 —)%
dX
dR
AR = ±(0.05 + 0.008R + 0.2 — ) %
dX
AL* 0.21
Aa* 0.20
Ab* 0.46
AE* 0.54
All uncertainties are at the 95% confidence level. All percentages are with
respect to the 100% level and not the reflectance value. Approximately half
-25
6.5 Certified Individual Reference Values and their Uncertainties
The NPL calibration data for tile No 126 was provided in terms of the CIE
(9)
L*,a*,b* Systenr . It was therefore, necessary to convert the data for
The NPL data could then be compared directly with the Ceram Research
Table 11 NPL and Ceram Research data for Master Tile GM89
L a b
The differences were used to correct the Ceram Research measurements (4.2) on
all the tiles, bringing their L,a,b values into line with the NPL calibration
on the Master Tile. Labels were printed by the computer giving the individual
calibration values for each tile - values which are directly traceable to the
NPL calibration.
The uncertainties in the colour values expressed relative to the master tile
can be derived from the repeatability of the colorimeter used to determine the
individual values after allowance for the small effect arising from different
The overall uncertainties (uC) on the certified L,a,b values are estimated by
of the master tile and the uncertainties on L,a,b when expressed relative to
26
These uncertainties are compared in Table 12. In each case they are expressed
In practice, the uncertainties expressed with respect to the master tile will
determine the agreement between colorimeters calibrated with tiles from the
stressed that they are marginally smaller than the overall uncertainties given
above.
These calibration data are suitable for most users of the Tomato Reference
reading in Hunter L,a,b values. If other data are needed these may be
required.
-27-
7 INSTRUCTIONS FOR USE
7.1.1 Store the reference tile at room temperature in the box provided. Do
7.1.2 Avoid scratching the glaze surface when handling or cleaning the tile.
7.1.3 Clean the tile by breathing on the glaze surface and drying off with a
7.1.4 Should the tile become badly soiled, gently wipe the glaze surface
To calibrate the colorimeter use the certified values issued with the tile.
For optimum repeatability always use the tile with the same orientation.
instructions.
28-
NB Avoid excessive exposure to heat during calibration to minimise thermo-
chromic effects (see 3.5). Do not expose the tile within the instrument for
-29
ANNEX A A METHOD FOR THE COLOUR MEASUREMENT OF UNSALTED TOMATO PASTE/
A.l Introduction
means of a tomato paste colour reference tile which has a colour typical of
that required by the tomato processing industry and their customers. This
A.3 Materials
A.4 Apparatus
diameter is recommended.
(25 °C preferably).
31 -
A.4.3 BCR Tomato Paste Colour Reference tile maintained at constant
A.4.A Optically clear glass specimen cell, diameter 62.5 mm, height 62.5 mm
A.4.5 Empty container approximately 100 mm internal diameter and 140 mm high
A.5.1 Preparation of test sample: Determine the total soluble solids (£TSS)
force the serum through the cloth. Reject the first ten drops and
allow two or three drops to fall onto the prism of the refractometer.
reading is obtained.
-32-
A.5.3 Test Sample: for measurement of the colour, a net weight of 300 g of
12.3
Vp = x 300
%TSS
(12.3 rather than 12.0 to allow for the fact that the percentage of
this proportion.)
A.5.3.1 Weigh Wp.g of laboratory sample paste into a 400 ml beaker. The
subsequent steps.
amounts and stir after each addition to break, up any lumps. DO NOT
ENTRAP AIR IN THE MIX. As the weight of the test sample approaches
and check the X TSS. Should the test sample be too dilute, DO NOT
A.6 Procedure
-33-
A.6.2 An instrument should be used which has an aperture of 50 mm nominal
A.6.3 Set the colorimeter to a zero scale reading by placing a black tile
supplied for zero adjustment over the aperture and make the zero
A.6.A To calibrate the instrument on the BCR Tomato. Paste Colour Reference
system is required. Place the tile over the aperture, without using
a glass plate and adjust the instrument to the L,a,b values of the
possible.
A.6.5 Introduce sufficient of the prepared sample into the sample cell, the
give a minimum depth of 20 mm. Place the light shield over the sample
possible.
A.6.6 The instrument should be zeroed and calibrated using the BCR tile at
-34
ANNEX B INTERCOMPARISON OF LABORATORIES AND INSTRUMENTS
B.l Participants
-35
AB Slotts, Uppsala, Sweden
During manufacture of the tile a small auxiliary firing was made to produce
50 tiles with high a values. These were to serve as Tile B in the experiment
described below.
Some 400 tiles were rejected at production (3.4) as being outside the limits
tiles were chosen from the further discards mentioned in 4.2 (Tile A) and from
36
the special production batch mentioned above (Tile B). These pairs of tiles
Tile B using their normal measurement procedure but without any intervening
glass plate if that was normally used. Measurements were then made on the
same tile using Tile A as a reference tile with the given values. Single
B.3 Results
that had been. In Figures Bla and Bib the results for a/b ratios are plotted
values from the 'true' values are quantised and the distribution of these
differences around zero is plotted. Note how for. the data using normal
procedures (Fig Bla), the data for Tile B are distributed much more widely
than when the Tile A is used as a reference (Fig Bib). This kind of result is
seen for all the variables and is summarised in Table Bl. Because the
deal in terms of the interquartile range of the data rather than their
-37
(a) 100 T
90 4
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- 80 4
L
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70 -•
CO
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JQ 60 •■
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50 -•
<D 40 -•
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Q.
to -■
3-3-1
-1.2 -1.0 -0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4
(b) 100 T
90 -•
<0
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L
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70 ■•
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38-
considerably reduced when the reference tile A is used. Mean and median also
approach closer to zero ie the measurements are closer to the 'true' values.
Since however the normal method for some participants was apparently to use a
those laboratories (of which there were 23) and to perform the same kind of
interquartile range for the complete set of data and for the subset of methods
Table Bl
Number of Interquartile
Vari able measurements Mean Median range
39-
Table B2
Number of Interquartile
Variable measurements Mean Median range
40-
REFERENCES
1 Jowitt, R., Escher, F., Kent, M., McKenna, B. and Roques, M. (1987)
London.
6 Malkin, F. and Verrill, J.F. (1983) in J. Schanda (Ed) Proc. CIE 20th
-41
CIE International Commission on Illumination. Recommendations on Uniform
42-
European Communities — Commission
ISBN 92-826-2403-X
The homogeneity of the batch of tiles is discussed and the results of a study
which confirms the stability of the tiles are presented. Details are given of
the procedure used to establish the certified values for individual tiles.
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