Você está na página 1de 5

WARNING! All paper copies are uncontrolled.

The controlled copy of this document is available at http://nexus.smri.org/Departments/Quality


This paper copy printed: 27 May 2014
Page 1 of 5

SUGAR MILLING RESEARCH INSTITUTE NPC


Subject:

TEST METHODS
DETERMINATION OF THE COLOUR AND TURBIDITY OF
WHITE SUGAR IN SOLUTION

Quality Manager

Approving Officer:
1.
Scope

Signature:

Section 8.6
Document No.
TM025
Rev No D
Effective Date
March 2013

This method is used for the determination of the colour and turbidity of white sugar in
solution.
2.

Field of Application
The method can be applied to all crystalline or powered white sugars, provided that a filtered
test solution can be prepared by the procedure specified in the method. The non-pH method
can only be used for sugars of colour of 50 ICUMSA units or less.

3.

Definitions

3.1

Transmittance of a solution - If I1, represents the radiant energy incident upon the first
surface of the solution and I2 represents the radiant energy leaving the second surface of the
solution. Then:T

3.2

transmittance of the solution (100 T = percentage

Tsoln/Tsolv

transmittancy of the solution

absorbancy of the solution

Absorbance (extinction)
As

3.4

Transmittancy - Let Tsoln represent the transmittance of a cell containing the solution and let
Tsolv represent the transmittance of the same or duplicate cell containing the pure solvent.
Then:
T1

3.3

=
I2/I1
transmittance)

log10Ts

Absorbancy index (extinction index) - Let b represent the length, (mm), of the absorbing
path between the boundry layers of the solution and let c represent the concentration, (g/cm 3),
of the sugar solution, Then:
As

As
bc

absorbancy index of the solution

3.5

ICUMSA colour - The value of the absorbancy index multiplied by 10 000 is reported as
ICUMSA colour. The resulting values are designated as ICUMSA units (IU), but since
measurements are made at a wavelength of 420 nm the value is designated as the ICUMSA
420 colour.

4.

Principle

WARNING! All paper copies are uncontrolled.


The controlled copy of this document is available at http://nexus.smri.org/Departments/Quality
This paper copy printed: 27 May 2014
Page 2 of 5

SUGAR MILLING RESEARCH INSTITUTE NPC


Subject:

TEST METHODS
DETERMINATION OF THE COLOUR AND TURBIDITY OF
WHITE SUGAR IN SOLUTION

Section 8.6
Document No.
TM025
Rev No D
Effective Date
March 2013

Approving Officer:
Quality Manager
Signature:
White sugar is dissolved in distilled water to give a solution of 30Bx or 50Bx. Some of this
solution is filtered through a membrane filter to remove turbidity while the remainder is
retained. Both the filtered and unfiltered solutions are adjusted to pH = 7 0,02 (or not
depending on the final colour of the solution) using either hydrochloric acid (approximately
0,005 M) or sodium hydroxide (approximately 0,005 M). The absorbances of both of these
solutions are measured at a wavelength of 420 nm and the ICUMSA 420 colour and the
turbidity are calculated.
5.

Reagents
Use only reagents of recognized analytical grade and only distilled water or water of
equivalent purity. The water quality must be greater than 90% removal of ionisable material
ie. >90%
A or B grade glassware may be used.
WARNING: Exercise care when preparing and using the following solutions. Goggles
and acid resistant gloves should be worn.

5.1

Hydrochloric acid 1 M - Measure 98 cm3 concentrated hydrochloric acid and dilute to 1000
cm3 in a volumetric flask.

5.2

Hydrochloric acid 0,005 M - Pipette 1 cm3 of 1 M hydrochloric acid into a 200 cm3
volumetric flask and make to volume with distilled water.

5.3

Sodium hydroxide 1 M - Weigh 40,0 g sodium hydroxide pellets and dissolve in some
distilled water. Cool the solution and then dilute to 1000 cm3 in a volumetric flask.

5.4

Sodium hydroxide 0,005 M - Pipette 1 cm3 1 M NaOH into a 200 cm3 volumetric flask and
make to volume with distilled water.

6.

Apparatus

6.1

Spectrophotometer - Capable of light transmission measurements at a wavelength of 420 nm


with the lowest practical bandwidth, e.g. 10 nm.

6.2

Optical glass cells - Glass cells of at least 50 mm in length should be used.

6.3

Membrane filters - Cellulose nitrate, pore size 0,45 m, 50 mm or 47 mm

6.4

Buchner funnels - Porcelain - 50-65 mm

6.5

Buchner flask - 500 cm3 capacity with rubber bungs to fit

6.6

Beakers - 250 cm3, 100 cm3 or 50 cm3

WARNING! All paper copies are uncontrolled.


The controlled copy of this document is available at http://nexus.smri.org/Departments/Quality
This paper copy printed: 27 May 2014
Page 3 of 5

SUGAR MILLING RESEARCH INSTITUTE NPC


Subject:

TEST METHODS
DETERMINATION OF THE COLOUR AND TURBIDITY OF
WHITE SUGAR IN SOLUTION

Approving Officer:
Quality Manager
6.7
Measuring cylinder - 100 cm3

Signature:

Section 8.6
Document No.
TM025
Rev No D
Effective Date
March 2013

6.8

Watch glass - 60 mm

6.9

Refractometer - Bench type

6.10

pH meter - Calibrated to two points (Buffers 4 and 7)

6.11

Magnetic stirrer - With follower

6.12

Laboratory balance - Readable to 0,01 g

7.

Procedure

7.1

Sample preparation - Mix the sample of sugar thoroughly. Weigh 40 0, 02 g (30 0,02 g
if only colour is required) of the sample into a 250 cm 3 beaker, add 90 cm3 (70 cm3 if only
colour is required) of distilled water and dissolve the sugar at room temperature using a
magnetic stirrer. In the case of 50Bx solution, 50g of thoroughly mixed sugar should be
weighed and dissolved in 50g of distilled water. Filter a portion of the solution through a 0,
45 m membranes under vacuum and label S1. Label the remaining unfiltered portion S2.
(Read the filtered and unfiltered samples absorbancies and brix and calculate the colour and
turbidity as shown below in the calculations. If the colour of the solution is 50 units or less
then this result will be reported as the sugar colour and turbidity respectively. If not proceed
with the method.) Adjust both these solutions to a pH of 7 0,02 using hydrochloric acid or
sodium hydroxide if the colour is above 50 IU. Measure the absorbancies at 420 nm on the
spectrophotometer using distilled water as a blank. Measure the refractometer brix of these
solutions.
Note: (1) A two point calibration of the pH meter i.e. pH 4 and7 should be done before
pH adjustment.
(2)Read the absorbance of the unfiltered portion S2 immediately off the
spectrophotometer as settling particles could give a false lower turbidity measurement.

8.

Expression of Results

8.1 Use the Brix reading at 20.0C to obtain the concentration of total solids in g/cm3 using the
formula indicated below.

Total solids (g/cm3)

Brix (a + b Brix + c Brix2 + d Brix3 + e Brix 4 )


100

WARNING! All paper copies are uncontrolled.


The controlled copy of this document is available at http://nexus.smri.org/Departments/Quality
This paper copy printed: 27 May 2014
Page 4 of 5

Section 8.6

SUGAR MILLING RESEARCH INSTITUTE NPC


Subject:

TEST METHODS
DETERMINATION OF THE COLOUR AND TURBIDITY OF
WHITE SUGAR IN SOLUTION

Approving Officer:
Quality Manager
where a
=
0.9971843

Signature:

3.8573810-3

1.25491610-5

8.12565910-8

5.61145510-10

ICUMSA 420 Colour

A s 10 000
bc

where As

Document No.
TM025
Rev No D
Effective Date
March 2013

absorbance at 420

nm (AU)
b
c

cell length (mm)


concentration of total solids (g/cm3)

Report results in ICUMSA Units (IU) to the nearest 10 units.


9. Example
Obtain the concentration of total solids in g/cm3 from the Brix reading at 20.0C using the equation in
8.1(or Table 2 in Appendix A).
Unfiltered solution:
Brix at 20.0C

31.1Bx

Concentration of total solids

0.352 g/cm3

Absorbance at 420 nm

0.117 AU

ICUMSA 420 colour

0.117 AU 10 000
50 mm 0.352 g/cm3

67.0 IU

Brix at 20.0C

31.1Bx

Concentration of total solids

0.352 g/cm3

Absorbance at 420 nm

0.091 AU

Filtered solution:

WARNING! All paper copies are uncontrolled.


The controlled copy of this document is available at http://nexus.smri.org/Departments/Quality
This paper copy printed: 27 May 2014
Page 5 of 5

SUGAR MILLING RESEARCH INSTITUTE NPC


Subject:

TEST METHODS
DETERMINATION OF THE COLOUR AND TURBIDITY OF
WHITE SUGAR IN SOLUTION

Approving Officer:

Quality Manager

ICUMSA 420 colour

Signature:
=

Section 8.6
Document No.
TM025
Rev No D
Effective Date
March 2013

0.091 AU 10 000
50 mm 0.352 g/cm3

50.7 IU

Unfiltered Colour - Filtered Colour

(67.0 - 50.7) IU

Report as 51 IU
Turbidity

=
9.

16.3 IUReport as 16 IU

Precision

The tolerance between duplicates 3 ICUMSA units. .


10.

Declaration
The method is suitable for its intended use.11.

Bibliography

11.1

ICUMSA Method Book Method GS2/3-10 (2007).

11.2

Laboratory Manual for South African Sugar Factories - 3rd Edition p 337.

11.3

Schoonees BM and Govender CN (2002), SMRI Technical Report No 1893, 24 October.

Você também pode gostar