GB 31604.47-2016 English PDF

GB 31604.47-2016: Food contact materials for export -- Paper and paper products -- Determination of fluorescent brightener -- Liquid chromatography
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GB 31604.47-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Food Contact Materials
and Articles – Determination of Fluorescent Brightener in
Paper, Paperboards and Paper Products
食品接触材料及制品 纸, 纸板及纸制品中荧光增白剂
ISSUED ON. SEPTEMBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
3. No action is required - Full-copy of this standard will be automatically and
immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3 
1 Application Scope ... 4 
2 Principle ... 4 
3 Reagents and Materials ... 4 
4 Apparatus ... 5 
5 Analytical Procedure ... 6 
6 Expression of Analytical Results ... 8 
Foreword
This Standard replaces the fluorescent substance testing part of GB/T 5009.78-2003,
Method for Analysis of Hygienic Standard of Papers for Food Packaging, and SN/T
2901-2011, Food Contact Materials for Export – Determination of Fluorescent Brighter
in Paper and Paper Products - Liquid Chromatography.
Compared with GB/T 5009.78, the major changes of this Standard are as follows.
-- it changes the standard name into “National Food Safety Standard – Food
Contact Materials and Articles – Determination of Fluorescent Brightener in Paper,
Paperboards and Paper Products”;
-- it adds confirmatory test;
-- it adds application scope.
National Food Safety Standard – Food Contact Materials
and Articles – Determination of Fluorescent Brightener in
Paper, Paperboards and Paper Products
1 Application Scope
This Standard specifies the method for the determination of fluorescent brighter in
food-contact paper, paperboards and paper products.
This Standard applies to the determination of fluorescent brighter in food-contact paper,
paperboards and paper products.
2 Principle
After fluorescent brighter absorbs near ultraviolet light (of wavelength 300 nm ~ 400
nm), the electrons in molecules transition from the ground state, return to the ground
state within extremely short time and give off blue or violet fluorescent light (of
wavelength 420 nm ~ 480 nm). Therefore, it is determined whether specimen contains
fluorescent brighter through observation of whether specimen has fluorescence under
the irradiation of an ultraviolet lamp of wavelength 365 nm. If specimen shows multiple
discontinuous small fluorescence spots or specimen has fluorescence but not
conspicuous, extract with an alkaline extracting solution, adjust the extracting solution
to acidity, use gauze to absorb fluorescent brighter in the extracting solution, and
observe whether the gauze has conspicuous fluorescent light under an ultraviolet lamp
of wavelength 365 nm in order to confirm whether specimen contains fluorescent
brighter.
3 Reagents and Materials
Unless specified otherwise, all reagents used for this method are analytically pure and
the water is of grade 1 water specified in GB/T 6682. All reagents and materials used
shall have no fluorescent light under an ultraviolet lamp.
3.1 Reagents
3.1.1 Acetonitrile (CH3CN). chromatographically pure.
3.1.2 Triethylamine [(CH3CH2)3N].
In a dark room or dark box, turn on the power switch of ultraviolet lamp and choose
the test wavelength of 365 nm. Placed the test pieces of 100 cm2 prepared about 20
cm from the ultraviolet light source; observe whether they have conspicuous blue or
violet fluorescent light. If specimen shows multiple discontinuous small fluorescence
spots or specimen has fluorescence but not conspicuous, it requires the execution of
the operating steps specified in 5.3 for confirmatory test.
5.3 Confirmation of fluorescent brighter
5.3.1 Preparation of standard control gauze
Weigh 2.0 g (accurate to 1 mg) of blank paper specimen pulverized uniformly in the
operating step of 5.1 to place into a 250 mL conical flask; add 0.5 mL of 40.0 μg/mL
C.I.220 standard solution, equivalent to that the content of C.I.220 in paper specimen
is 10 mg/kg; add 100 mL of alkaline extracting solution (of volume ratio of acetonitrile,
water and triethylamine 40.60.1) under dark conditions (of illuminance less than 20 Lux
required); perform supersonic extraction for 40 min at 50°C. Cool to room temperature
after the completion of extraction; filter the extracting solution through a glass funnel
containing a small amount of glass wool (no fluorescent brighter contained) to a
chicken-shaped flask or obtain clarified extracting solution by centrifugation (for 5 min
at the rotational speed of 3 500 r/min). Perform vacuum concentration of the extracting
solution to about 40 mL ~ 50 mL at 50°C; transfer the concentrated solution to a 250
mL beaker; after using water to wash the chicken-shaped flask, transfer to a 250 mL
beaker along with washings; use hydrochloric acid (of volume fraction 10%) to adjust
the pH value to 3 ~ 5; add water dropwise to about 100 mL. Then immerse one piece
of gauze of 5 cm × 5 cm in the extracting solution and absorb on a water bath for 30
min at 40°C. Use tweezers to take out the gauze; use hand to squeeze out most of
liquid; fold the gauze into 4 layers with the area of each layer 2.5 cm × 2.5 cm; place
on a watch glass.
5.3.2 Specimen extraction and absorption
Weigh 2.0 g (accurate to 1.0 mg) of specimen pulverized uniformly in the operating
step of 5.1 to place into a 250 mL conical flask; the other operating steps are as
specified in the step of 5.3.1, “add 100 mL of alkaline extracting solution (of volume
fraction of acetonitrile, water and triethylamine 40.60.1) under dark conditions (of
illuminance less than 20 Lux required) ... place on a watch glass”. Two parallel tests
shall be performed for each specimen.
5.3.3 Blank test
Use 2.0 g of water to replace specimen and perform tests in accordance with the
operating steps of 5.3.2.
5.3.4 Determination of fluorescent brighter
In a dark room or dark box, turn on the power switch of ultraviolet lamp and choose
the test wavelength of 365 nm. Placed the watch glasses of standard control gauze,
GB 31604.47-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Food Contact Materials
and Articles – Determination of Fluorescent Brightener in
Paper, Paperboards and Paper Products
食品接触材料及制品 纸, 纸板及纸制品中荧光增白剂
ISSUED ON. SEPTEMBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
3. No action is required - Full-copy of this standard will be automatically and
immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3 
1 Application Scope ... 4 
2 Principle ... 4 
3 Reagents and Materials ... 4 
4 Apparatus ... 5 
5 Analytical Procedure ... 6 
6 Expression of Analytical Results ... 8 
Foreword
This Standard replaces the fluorescent substance testing part of GB/T 5009.78-2003,
Method for Analysis of Hygienic Standard of Papers for Food Packaging, and SN/T
2901-2011, Food Contact Materials for Export – Determination of Fluorescent Brighter
in Paper and Paper Products - Liquid Chromatography.
Compared with GB/T 5009.78, the major changes of this Standard are as follows.
-- it changes the standard name into “National Food Safety Standard – Food
Contact Materials and Articles – Determination of Fluorescent Brightener in Paper,
Paperboards and Paper Products”;
-- it adds confirmatory test;
-- it adds application scope.
National Food Safety Standard – Food Contact Materials
and Articles – Determination of Fluorescent Brightener in
Paper, Paperboards and Paper Products
1 Application Scope
This Standard specifies the method for the determination of fluorescent brighter in
food-contact paper, paperboards and paper products.
This Standard applies to the determination of fluorescent brighter in food-contact paper,
paperboards and paper products.
2 Principle
After fluorescent brighter absorbs near ultraviolet light (of wavelength 300 nm ~ 400
nm), the electrons in molecules transition from the ground state, return to the ground
state within extremely short time and give off blue or violet fluorescent light (of
wavelength 420 nm ~ 480 nm). Therefore, it is determined whether specimen contains
fluorescent brighter through observation of whether specimen has fluorescence under
the irradiation of an ultraviolet lamp of wavelength 365 nm. If specimen shows multiple
discontinuous small fluorescence spots or specimen has fluorescence but not
conspicuous, extract with an alkaline extracting solution, adjust the extracting solution
to acidity, use gauze to absorb fluorescent brighter in the extracting solution, and
observe whether the gauze has conspicuous fluorescent light under an ultraviolet lamp
of wavelength 365 nm in order to confirm whether specimen contains fluorescent
brighter.
3 Reagents and Materials
Unless specified otherwise, all reagents used for this method are analytically pure and
the water is of grade 1 water specified in GB/T 6682. All reagents and materials used
shall have no fluorescent light under an ultraviolet lamp.
3.1 Reagents
3.1.1 Acetonitrile (CH3CN). chromatographically pure.
3.1.2 Triethylamine [(CH3CH2)3N].
In a dark room or dark box, turn on the power switch of ultraviolet lamp and choose
the test wavelength of 365 nm. Placed the test pieces of 100 cm2 prepared about 20
cm from the ultraviolet light source; observe whether they have conspicuous blue or
violet fluorescent light. If specimen shows multiple discontinuous small fluorescence
spots or specimen has fluorescence but not conspicuous, it requires the execution of
the operating steps specified in 5.3 for confirmatory test.
5.3 Confirmation of fluorescent brighter
5.3.1 Preparation of standard control gauze
Weigh 2.0 g (accurate to 1 mg) of blank paper specimen pulverized uniformly in the
operating step of 5.1 to place into a 250 mL conical flask; add 0.5 mL of 40.0 μg/mL
C.I.220 standard solution, equivalent to that the content of C.I.220 in paper specimen
is 10 mg/kg; add 100 mL of alkaline extracting solution (of volume ratio of acetonitrile,
water and triethylamine 40.60.1) under dark conditions (of illuminance less than 20 Lux
required); perform supersonic extraction for 40 min at 50°C. Cool to room temperature
after the completion of extraction; filter the extracting solution through a glass funnel
containing a small amount of glass wool (no fluorescent brighter contained) to a
chicken-shaped flask or obtain clarified extracting solution by centrifugation (for 5 min
at the rotational speed of 3 500 r/min). Perform vacuum concentration of the extracting
solution to about 40 mL ~ 50 mL at 50°C; transfer the concentrated solution to a 250
mL beaker; after using water to wash the chicken-shaped flask, transfer to a 250 mL
beaker along with washings; use hydrochloric acid (of volume fraction 10%) to adjust
the pH value to 3 ~ 5; add water dropwise to about 100 mL. Then immerse one piece
of gauze of 5 cm × 5 cm in the extracting solution and absorb on a water bath for 30
min at 40°C. Use tweezers to take out the gauze; use hand to squeeze out most of
liquid; fold the gauze into 4 layers with the area of each layer 2.5 cm × 2.5 cm; place
on a watch glass.
5.3.2 Specimen extraction and absorption
Weigh 2.0 g (accurate to 1.0 mg) of specimen pulverized uniformly in the operating
step of 5.1 to place into a 250 mL conical flask; the other operating steps are as
specified in the step of 5.3.1, “add 100 mL of alkaline extracting solution (of volume
fraction of acetonitrile, water and triethylamine 40.60.1) under dark conditions (of
illuminance less than 20 Lux required) ... place on a watch glass”. Two parallel tests
shall be performed for each specimen.
5.3.3 Blank test
Use 2.0 g of water to replace specimen and perform tests in accordance with the
operating steps of 5.3.2.
5.3.4 Determination of fluorescent brighter
In a dark room or dark box, turn on the power switch of ultraviolet lamp and choose
the test wavelength of 365 nm. Placed the watch glasses of standard control gauze,