GB 31604.48-2016 English PDF (GB31604.48-2016)

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GB 31604.48-2016: Determination of formaldehyde for food packaging material
GB 31604.48-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National standard for food safety –
Food contact materials and products -
Determination of formaldehyde migration
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
Method I Acetylacetone spectrophotometric method ... 4
2 Principle ... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 5
5 Analysis steps ... 5
6 Expression of analysis results ... 6
7 Precision ... 7
8 Others ... 7
Method II Chromotropic acid spectrophotometric method ... 7
9 Principle ... 7
10 Reagents and materials ... 7
11 Analysis steps ... 9
12 Expression of analysis results ... 10
13 Precision ... 10
14 Others ... 10
Annex A Calibration of formaldehyde standard stock solution ... 12
Foreword
This Standard replaces GB/T 5009.178-2003 “Determination of formaldehyde for food
packaging material”, Clause 8 “Formaldehyde” in GB/T 5009.61-2003 “Method for
analysis of hygienic standard of products of tripolycyanamide for food packaging”,
Clause 7.2 “Free formaldehyde” in GB/T 5009.69-2008 “Method for analysis of
hygienic standard of epoxy phenolic coatings for inner wall of food cans” and
determination of formaldehyde in water-based simulants in GB/T 23296.26-2009
“Food contact materials - Polymer - Determination of formaldehyde and
hexamethylenetetramine in food simulants - Spectrophotometry”.
Compared with GB/T 5009.178-2003, the main changes of this Standard are as follows.
- MODIFY the standard name TO “National standard for food safety - Food contact
materials and products - Determination of formaldehyde migration”;
- DELETE the oscillopolarographic method; ADD acetylacetone spectrophotometric
method and chromotropic acid spectrophotometric method.
National standard for food safety –
Food contact materials and products –
Determination of formaldehyde migration
1 Scope
This Standard specifies the spectrophotometric method for the determination of
formaldehyde migration in food contact materials and products.
This Standard applies to the determination of formaldehyde migration in food contact
materials and products.
Method I Acetylacetone spectrophotometric method
2 Principle
After the food simulant is in contact with the sample, the formaldehyde in the sample
migrates to the food simulant. In the presence of ammonium acetate, gormaldehyde
reacts with acetylacetone and generate yellow 3,5-diacetyl-1,4 
dihydrodimethylpyridine; USE a spectrophotometer to measure the absorbance of the
test solution at 410 nm; COMPARE it with that of the reference series to obtain the
content of formaldehyde in the food simulant, and then obtain the formaldehyde
migration in the sample.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical reagent
and water is the tertiary water specified in GB/T 6682.
3.1 Reagents
3.1.1 Anhydrous ethanol (CH3CH2OH).
3.1.2 Anhydrous ammonium acetate (CH3COONH4).
3.1.3 Acetylacetone (C5H8O2).
3.1.4 Glacial acetic acid (CH3COOH). guarantee reagent.
3.1.5 Sodium hydroxide (NaOH).
3.2 Preparation of reagents
3.2.1 Water-based food simulants. PREPARE according to the specifications of GB
5009.156.
3.2.2 Acetylacetone solution. WEIGH 15.0 g of anhydrous ammonium acetate and
dissolve in the appropriate amount of water; TRANSFER into a 100 mL volumetric flask;
ADD 40 μL of acetylacetone and 0.5 mL of glacial acetic acid; DILUTE with water to
the scale; MIX well. This solution is prepared when it is in need.
3.3 Preparation of standard solutions
3.3.1 Formaldehyde solution (37 % ~ 40 %, mass fraction). preserve at 0 °C ~ 4 °C.
3.3.2 Formaldehyde standard stock solution. PIPETTE 5.0 mL of formaldehyde
solution to a 1000 mL volumetric flask; DILUTE with water to the scale; PRESERVE at
0 °C ~ 4 °C; it is valid for 12 months; CALIBRATE before use (see Annex A); or use
formaldehyde solution standard products to prepare directly.
3.3.3 Formaldehyde standard use solution. according to the calibrated formaldehyde
concentration, accurately transfer a certain volume of formaldehyde standard stock
solution to dilute with the corresponding simulants, respectively, to the equivalent of
10 mg formaldehyde per liter. This solution is prepared when it is in need.
4 Instruments and equipment
4.1 UV-visible spectrophotometer.
4.2 Constant-temperature water bath. the precision is controlled at ± 1 °C.
4.3 Colorimetric tube with stopper. 10 mL (with scale).
5 Analysis steps
5.1 Migration test
According to the intended use and the use conditions of the sample to be tested, in
accordance with the requirements of GB 5009.156 and GB 31604.1, carry out the
migration test to the sample. During the migration test to prior to the determination, it
shall pay attention to sealing, in order to avoid the loss of formaldehyde volatile. At the
same time carry out the blank test.
5.2 Chromogenic reaction
and water is a tertiary water or deionized water specified in GB/T 6682. All reagents in
which formaldehyde shall not be detected by this method.
10.1 Reagents
10.1.1 Anhydrous ethanol (CH3CH2OH).
10.1.2 Chromotropic acid (C10H8O8S2).
10.1.3 Sulfuric acid. guarantee reagent.
10.1.4 Glacial acetic acid (CH3COOH). guarantee reagent.
10.1.5 Sodium hydroxide (NaOH).
10.2 Preparation of reagents
10.2.1 Water-based food simulants. PREPARE according to the specifications of GB
5009.156.
10.2.2 Sulfuric acid solution. MEASURE 100 mL of sulfuric acid, DISSOLVE in 50 mL
of water, STIR slowly, MIX well.
NOTE. Concentrated sulfuric acid will produce a lot of heat when contacting with water, and the
density of concentrated sulfuric acid is greater than that of water, so adding water to
concentrated sulfuric acid may lead to bruising. During preparation, the sulfuric acid shall be
added slowly along the beaker wall to the water while stirring constantly.
10.2.3 Chromotropic acid solution (5 mg/mL). WEIGH 0.500 g of chromotropic acid;
DISSOLVE in the appropriate amount of water; TEANSFER into a 100 mL volumetric
flask; DILUTE with water to the scale; MIX and then filter with slow-speed filter paper;
COLLECT the filtrate for further use. This solution is prepared when it is in need.
10.3 Preparation of standard solutions
10.3.1 Formaldehyde solution (37 % ~ 40 %, mass fraction). preserve at 0 °C ~ 4 °C.
10.3.2 Formaldehyde standard stock solution. PIPETTE 5.0 mL of formaldehyde
solution to a 1000 mL volumetric flask; DILUTE with water to the scale; PRESERVE at
0 °C ~ 4 °C; it is valid for 12 months; CALIBRATE before use (see Annex A); or use
formaldehyde solution standard products to prepare directly.
10.3.3 Formaldehyde standard use solution. according to the calibrated formaldehyde
concentration, accurately transfer a certain volume of formaldehyde standard stock
solution to dilute with the corresponding simulants, respectively, to the equivalent of
10 mg formaldehyde per liter. This solution is prepared when it is in need.
Annex A
Calibration of formaldehyde standard stock solution
A.1 Reagents
A.1.1 Sodium hydroxide (NaOH).
A.1.2 Hydrochloric acid (HCl). 36.0 % ~ 38.0 %.
A.1.3 Iodine (I2).
A.1.4 Potassium Iodide (KI).
A.1.5 Soluble starch.
A.2 Preparation of reagents