•
ICUMSA
Method GS2/3/9-19 (2007)
The Determination of Insoluble Matter in
White Sugar by Membrane Filtration - Official1
1 Scope
The membrane filter method of Hibbert and Phillip
son2, modified by using a lower temperature 3.4, is used
to determine the amount of water-insoluble matter in
white sugars. This method has Official status for such
sugars1.
2 Field of Application
The method is applicable to all crystalline white sugars
(General Subject 2), powdered sugars that do not con
tain additives (General Subject 3) and plantation white
sugars (General Subject 9). For those sugars with poor
filtration characteristics a modified procedure is de
scribed below in section 6.3.
3 Principle
The sugar to be tested is dissolved in hot water and fil
tered through a membrane filter of pore size 8.0 µm.
The membrane and the retained insoluble matter are
thoroughly washed, dried and weighed.
The insoluble matter content is calculated from the in
crease in mass of the membrane filter.
4 Reagents
WARNING AND SAFETY PRECAUTIONS
USERS OF THIS METHOD ARE ADVISED TO
CONSULT THEIR NATIONAL HEALTH AND
SAFETY LEGISLATION BEFORE PREPARING
AND USING THE CHROMATOGRAPHIC SPRAY
REAGENT.
The water used must be deionised and purified by
membrane filtration (6.2). Its temperature must be 45
oc.
4.1 Chromatographic spray reagent - 1-naphthol/
phosphoric acid solution. Dissolve 1.0 g of 1-naphthol
in 100 mL of ethanol and add 10 mL of ortho-phos
phoric acid (p20 "" 1.69 g/mL).
NOTE - The ethanol used may be industrial methylated spirits con
taining 98-99% m/m total alcohols.
5 Apparatus
5.1 Membrane filters with hydrophobic rim - di
ameter about 50 mm, pore size 8.0 µm, e.g. Whatman
Schleicher and Schuell cellulose nitrate filter AE99,
Cat. No.10 405 079.
NOTE - Pore size is determined by 'bubble point' testing.5
5.2 Filtration apparatus - comprising a holder for
the membrane filter (5.1) fitted into a conical fil
tration flask, of capacity 4 L, connected with a
vacuum system.
5.3 Stainless steel jug - capacity 2 L with a stainless
steel stirring rod.
5.4 Tweezers.
5.5 Plastic Petri dishes.
5.6 Drying oven - maintained between 60 and 65 °C.
5.7 Analytical balance - readable to 0.1 mg.
5.8 Balance - capacity 5 kg, readable to 1 g.
6 Procedure
6.1 Preparation of water. Filter 5 L of water
through an 8 µm membrane filter prepared as in 6.2.
After the first 500 mL has filtered, tum off the vacuum.
Swirl this 500 mL around the flask and discard.
Continue the filtration of the remaining 4.5 L of water.
This water should be used for all requirements in steps
6.2 to 6.6. All equipment (jugs, stirring rods, tweezers)
should be rinsed in this filtered water before proceeding
further.
6.2 Preparation of membrane filter. Wash the
mem branes (5.1) by immersion in boiling distilled
water for 6 min; drain the excess water from the
membranes and transfer individually to clean, dry Petri
dishes (5.6) by using tweezers (5.5).
Dry the membranes in their dishes with the lids re
moved for 1 h at 60 °C to 65 °C in the drying oven.
After drying, replace the lids and cool for 30 min in a
desiccator. Record the mass of the cooled membranes
to the nearest 0.1 mg.
6.3 Preparation of sample solution.
Weigh
500 ± 1 g of the sample directly into the stainless steel
jug (5.4). If filtration turns out to be a problem, or sam
ple size is limiting, the sample mass may be reduced to
250 ± 1 g or further if required. Whilst accuracy is lost
when the sample size is reduced, this may be unavoida
ble.
Add hot distilled water at about 45 °C to the jug to give
a final volume of about 900 mL. Stir the mixture with
2007-04-26 GS2/3/9- l 9 (2007) page 1

,
 ICUMSA

the stainless steel rod, or a magnetic stirrer, and heat to

about 45 °C; continue stirring until all the sugar has
dissolved.
NOTE - Cloths for drying apparatus may be a serious source of con
tamination. It is therefore important that all apparatus should be rinsed
thoroughly with distilled water immediately prior to use and air dried
or oven dried, but not dried with a cloth.
6.4 Filtration of the sugar solution. Moisten a
weighed membrane filter by floating it on distilled wa
ter in the Petri dish. Place the moistened filter in the fil
ter holder (5.3) and pass the hot sugar solution through
the membrane filter under reduced pressure. Carefully
rinse the jug and stirring rod into the filter holder with
hot distilled water. Wash the retained insoluble matter
and the membrane in the filter holder using a total vol
ume of hot distilled wash water of about 500 mL.
NOTE - Do not allow air to be drawn through the membrane after
washing, because there may be a significant amount of particulate
matter in the atmosphere.
6.5 Drying and weighing of the membrane.
Return the membrane to its original Petri dish. Dry the
dish with the lid removed in the oven for 1 hour at 60
°C to 65 °C. Replace the lid and cool the dish for 30
min in a desiccator. Reweigh the membrane to
the nearest
0.1 mg.
8 Bibliography
1 Parkin G. (2006): Referee's Report, General Sub
ject 2, ICUMSA
2 Hibbert D. and Phillipson R.T. (1966): Int.
Sugar J., 68, 39-44
3 Cronewitz. T. and Serkezy W. (1973): Zucker 2.6..,.
134-138
4 Reinefeld E. and Schneider F., eds. (1983). Ana
lytische Betriebskontrolle der Zuckerindustrie.
Tei! C3 WeiBzucker, Bartens, Berlin, 25-28
5 Millipore Laboratory Catalogue (1991): Millipore
Intertech, Bedford, Mass., 9
9 Historical
The Hibbert and Phillipson method was Tentatively
adopted at the 15th Session in 1970. It was published as
a Tentative method, GS2/3-19, in the 1994 Methods
Book. At the 23rd Session in 2002 Method GS2/3-19
was adopted as Official for insoluble matter contents
greater than 10 mg/kg. In 2006 it was modified and
adopted as Official for all insoluble matter contents,
and including plantation white sugars, as Method
GS2/3/9-19.

The effectiveness of the washing is essential to the ac

curacy of the test. This may be checked by spraying oc
casional membranes, after use, with the 1-naphthol/
phosphoric acid chromatographic spray reagent (4.1),
and heating to 105 °C. The membrane should be entire
ly free of any trace of violet coloration.

7 Expression of Results
7.1 Calculation. The insoluble matter content of the
sugar expressed in milligrams of insoluble matter per
kilogram of sample is given by:

Insoluble matter (mg/kg) = . 106

where:
m1 = mass in grams of the membrane filter (6.2)
m2 = mass in grams of filter+insoluble matter
(6.6)
m0 = mass in grams of sample taken for test (6.3)

Express the result to the nearest mg/kg.

The amount of sample, used for the determination,

should always be reported with the results.

7.2 Precision. For white sugars, the absolute differ

ence between two results obtained under repeatability
conditions shall be not greater than 4.9 mg/kg. The ab
solute difference between two resu!ts obtained under
reproducibility conditions shall be not greater than 7.2
mg/kg.
GS2/3/9-19 (2007) page 2