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GB 31604.48-2016National standard for food safety - Food contact materials and products - Determination of formaldehyde migration (English PDF)

食品安全国家标准食品接触材料及制品甲醛迁移量的测定

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Issued by

National Health and Family Planning Commission of the People’s Republic of China

Level / Type

National · Mandatory

Issue date

October 19, 2016

Implementation date

April 19, 2017

Scope

GB 31604.48-2016 is the English-translated version of 食品安全国家标准食品接触材料及制品甲醛迁移量的测定.

GB 31604.48-2016 — 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

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Document preview — GB 31604.48-2016

National Standard of the People's Republic of China

Issued by: National Health and Family Planning Commission of the People’s Republic of China

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

3.2 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.

4 Instruments and equipment

4.1 UV-visible spectrophotometer.

4.2 Constant-temperature water bath. the precision is controlled at ± 1 °C.

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.

5.3 Plotting of standard curve

TAKE 7 10 mL colorimetric tubes; according to the type of simulants used in the

migration test, add corresponding formaldehyde standard use solution according to

Table 1;

5.4 Determination of sample solution and blank solution

PLACE the sample solution and the blank solution after chromogenic reaction into a

10 mm colorimetric cuvette; TAKE the blank solution after chromogenic reaction as the

reference;

6 Expression of analysis results

6.1 Calculation of formaldehyde concentration in food simulants

The concentration of formaldehyde in food simulants is calculated according to

equation (1)

7 Precision

The absolute difference between the two independent determination results obtained

under repeatability shall not exceed 10 % of the arithmetic mean.

8 Others

TAKE the concentration value corresponding to the absorbance of 0.01 higher than

the absorbance value of the blank solution AS the detection limit;

9 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 sulfuric acid, gormaldehyde reacts

with chromotropic acid and generate purple compounds; USE a spectrophotometer to

measure the absorbance of the test solution at 574 nm;

10 Reagents and materials

Unless otherwise stated, the reagents used in this method are of analytical reagent

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

10.2 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.

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.

11 Analysis steps

11.1 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.

11.2 Blank test

In addition to not contact with the sample to be tested, carry out the blank test

according to 11.1.

immediately in an ice-water bath for 2 min; TAKE out and return to room temperature.

11.4 Working curve

TAKE 6 10 mL colorimetric tubes; according to the type of simulants used in the

migration test, add corresponding formaldehyde standard use solution according to

Table 2; ADD corresponding simulant to 1.0 mL; ADD 1.0 mL of colorimetric acid

solution respectively; ADD slowly 8.0 mL of sulfuric acid solution; carefully shake

colorimetric tubes. After the solution is sufficiently shaken, place the colorimetric tubes

in a 90 °C water bath for 20 min; COOL immediately in an ice-water bath for 2 min;

TAKE out and return to room temperature.

12 Expression of analysis results

12.1 Calculation of formaldehyde concentration in food simulants

The concentration of formaldehyde in food simulants is calculated according to

equation (2)

13 Precision

The absolute difference between the two independent determination results obtained

under repeatability shall not exceed 10 % of the arithmetic mean.

......

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 12 pages — is available in the English PDF.

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