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These were:

1. It is recommended to carry out further tests with the glass frits that show a surface like crystal sugar
to find an alternative to the Braunschweig colour-type standards for method GS2-13. The tests should
consider both reflectance ratios R(426)/R(620) and R(495)/R(620) with the aim to concentrate on one
reflectance ratio in the future.
2. It is recommended to continue the studies on turbidity measurement and to enclose the calibration
procedure with formazin standards to the planned collaborative test. (Due to the potential
carcinogenicity of hydrazinium sulphate used to prepare the formazin standards, it will be necessary
to change the method for the ring test using an alternative non-toxic reagent).

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The activities to find a stable alternative material for calibration of reflexometers for determination of the
colour-type of white sugar were continued. Presently the ICUMSA method GS2-13 (1998) uses two sugar
standards (colour-type “0” and colour-type “6”) from the Braunschweig Scale for calibration of the
instrument. The sugar standards are produced in a time-consuming procedure by InnoSweet GmbH
Braunschweiga.
In 2004 a comparative test with 9 participants was carried out to evaluate if sintered glass frits with a
surface like crystal sugar could be a potential alternative to the sugar standards (for the participating
laboratories see Appendix 1, Table 1). The comparative test included the determination of the colour-type
according to ICUMSA method GS2-13 of 6 sugar samples after calibrating the reflexometer with sugar
standards, with sintered glass frits and, if available, with ceramic tiles. In the first part of the comparative

a
Successor of Nordzucker InnoCenter GmbH and Institut für Technologie der Kohlenhydrate an der TU
Braunschweig

1
test the calibration values of the standard materials were based on the reflectance ratio R(426)/R(620). In
the second part of the comparative test the calibration values of the standard materials were given on the
basis of the reflectance ratio R(495)/R(620). The calibration values for the sugar standards and the
sintered glass frits were determined by InnoSweet GmbH (ICUMSA method GS2-13, apparatus: Elrepho,
Carl Zeiss, Jena) and for the ceramic tiles by Dr. Kernchen GmbH (apparatus: PMQ3/RA3). For
determination of the colour-type after calibration with the different standard materials a “Sucroflex”
reflexometer (Dr. Kernchen GmbH) or a “Saccharoflex” reflexometer (Schmidt & Haensch) were
applied.
The resulting mean values for the colour-type of the sugar samples after calibration with the different
standard materials are shown in Appendix 1, Figure 1.

When the calibration values for the sugar standards and the glass frits are given on the basis of the
reflectance ratio R(426)/R(620) the calibration with the glass frits leads to slightly lower colour-types for
the analysed sugar samples. When the calibration values on the basis of the reflectance ratio
R(495)/R(620) are applied the calibration with the glass frits gives comparable results for the colour-type
compared to that obtained using sugar standards for sugar samples with colour-types up to 1.5 CTU.
According to ICUMSA method GS2-13 there is almost no difference between the calibration values for
the sugar standards depending on the reflectance ratio they were derived from. But for the coloured glass
frits, used for calibration of the reflexometer instead of sugar standard “6”, a significantly higher
calibration value is obtained on the basis of the reflectance ratio R(495)/R(620) compared to that obtained
on the basis of the reflectance ratio R(426)/R(620). This causes the increasing deviation between the
analysed colour-type when calibrated with glass frits or sugar standards for samples with colour-types
higher than 1.5 CTU.
According to Figure 1, Appendix 1 also the calibration of the reflexometer with ceramic tiles yields
comparable results to those obtained with sugar standards. But here the data are based on the results of
only 3 participants.

A collaborative study is planned to evaluate the precision of the determination of reflectance

measurement with glass frits and ceramic tiles compared to the Braunschweig colour-type standards. The
study should be based on a higher number of participants as in the prior comparative test. Furthermore
there should be an equal number of participants with a “Sucroflex”reflexometer (Dr. Kernchen GmbH)
and a “Saccharoflex” reflexometer (Schmidt & Haensch) to avoid an influence by the instrument used. In
the collaborative study the calibration values for the standard materials will be given on the basis of the
reflectance ratio R(495)/R(620). Prior to the study the stability of the glass frits will be checked.

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Turbidity is an important parameter for sugar quality. At present there is no ICUMSA method for
turbidity determination in white sugar. The determination of turbidity by measuring the difference of the
colour of a sugar solution before and after 0.45 µm membrane filtration is widespread in the sugar
industry. The International Society of Beverage Technologists (ISBT) fixed this method in the guidelines
for granular sucrose. In a preliminary study from SPRI and Pepsi, presented by M. A. Godshall, Referee
of Subject 3, at the 24th Interim meeting in Atlanta, the method was applied to six sugar samples. The
results showed a good precision of the method similar to those of the ICUMSA method GS2/3-10 for the
determination of white sugar solution colour. Furthermore the importance to specify the filter material for
the turbidity method was emphasised. Associate Referee M. Kuchejda introduced on the 24th Session a
calibration procedure with formazin standards to compensate for differences in the optical design of the
applied photometers. The calibration procedure includes the determination of the absorbancy of NTU
standards expressing the results in ICUMSA units. The slope of the obtained linear calibration curve is
used for the calculation of a correction factor which is multiplied by the analysed difference of the
solution colour of the filtered and unfiltered sugar solution.

2
Due to the potential carcinogenity of hydrazinium sulphate used to prepare the formazin standards M.
Kuchejda replaced the formazin standards in the calibration procedure by latex standards (AMCO AEPA-
1 turbidity standards)b. These standards consist of suspensions of submicron solid polymer beads
(PS/DVB-latex) suspended in ultra-pure water and have defined turbidity values within the range from 0 to
10 NTUc. Meanwhile M. A. Godshall started a collaborative study on the method for determination of
turbidity as colour of a white sugar solution before filtration and after filtration. The participants were
requested to perform the calibration procedure on an optional basis. The results will be presented at the
25th Session.
A Recommendation on this matter will be given on the basis of the results of the collaborative study.

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The Referee gratefully acknowledges all the participants taking part in the comparative test on reflectance
measurement: J. van Eekelen, F. Führer, Dr. W. Kernchen, M. Kuchejda, Dr. R. Lemmes, G. Parkin, Dr.
G. Pollach, Dr. H. Puke.
Furthermore the Referee gratefully acknowledges M. A. Godshall for organisation of the collaborative
study on the determination of the turbidity in white sugar.



























b
GFS Chemicals, Inc. David K. Baust PO Box 245 3041 Home Rd. Powell, OH 43065 USA
c
nephelometric turbidity units

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Agrana Zucker GmbH, Leopoldsdorf, Austria
British Sugar PLC, Petersborough, Great Britain
Cosun Food Technology Centre, Roosendaal, Netherlands
InnoSweet GmbH, Braunschweig, Germany
Dr. W. Kernchen, Seelze, Germany
Pfeifer & Langen, ETA Elsdorf, Elsdorf, Germany
Schmidt & Haensch GmbH, Berlin, Germany
Südzucker AG, ZAFES Offstein, Obrigheim, Germany
Zuckerforschung Tulln Gesellschaft m.b.H, Tulln, Germany



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