GB 31604.49-2023 PDF English
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National food safety standard - Food contact materials and products - Determination of multi-elements and determination of multi-element migration
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| GB 31604.49-2016 | English | 85 |
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National food safety standard -- Food contact materials and articles -- Migration of arsenic, cadmium, chromium, nickel, lead, antimony and zinc
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GB 31604.49-2023: National food safety standard - Food contact materials and products - Determination of multi-elements and determination of multi-element migration
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Products - Determination of Multi-elements and
Determination of Multi-element Migration
Issued on: SEPTEMBER 6, 2023
Implemented on: MARCH 6, 2024
Issued by. National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 4
1 Scope... 5
Part 1 - Determination of Arsenic, Cadmium, Chromium and Lead... 5
Method 1 Inductively Coupled Plasma Mass Spectrometry... 5
2 Principle... 5
3 Reagents and Materials... 5
4 Instruments and Equipment... 7
5 Analytical Procedures... 7
6 Expression of Analysis Results... 9
7 Precision... 10
8 Others... 10
Method 2 Inductively Coupled Plasma Optical Emission Spectrometry... 10
9 Principle... 10
10 Reagents and Materials... 11
1 Scope
This Standard specifies the method for the determination of arsenic, cadmium, chromium and
lead, and the determination of aluminum, arsenic, barium, cadmium, cobalt, chromium, copper,
iron, lithium, manganese, molybdenum, nickel, lead, antimony, tin and zinc migration in food
contact materials and products.
Part 1 is applicable to the determination of arsenic, cadmium, chromium and lead in food
contact paper and cardboard materials and products, cork stoppers and bamboo and wood
products.
Part 2 is applicable to the determination of aluminum, arsenic, barium, cadmium, cobalt,
chromium, copper, iron, lithium, manganese, molybdenum, nickel, lead, antimony, tin and zinc
migration in food contact plastic materials and products, food contact paints and coatings, food
contact rubber materials and products, inks for food contact materials and products, adhesives
for food contact materials and products, food contact paper and cardboard materials, pacifiers,
enamel products, ceramic products, glass products, food contact plastic resins, food contact
metal materials and products.
Part 1 - Determination of Arsenic, Cadmium, Chromium
and Lead
Method 1 Inductively Coupled Plasma Mass Spectrometry
2 Principle
After the specimen is crushed, use nitric acid for digestion. After the obtained solution is diluted
with water to a constant volume, adopt an inductively coupled plasma mass spectrometer to
conduct the determination. Take the specific mass number of the element (mass-to-charge ratio,
m/z) for qualitative analysis and the external standard method for quantitative analysis.
3 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all excellent-grade pure,
and the water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3). excellent-grade pure or higher.
3.1.2 Argon (Ar). argon ( 99.995%) or liquid argon.
3.1.3 Helium (He). helium ( 99.995%).
3.2 Preparation of Reagents
3.2.1 Nitric acid solution (5 + 95). measure-take 50 mL of nitric acid, slowly add it to 950 mL
of water and evenly mix it.
3.2.2 Nitric acid solution (1 + 4). measure-take 1 L of nitric acid, slowly add it to 4 L of water
and evenly mix it.
3.3 Reference Materials
3.3.1 Element standard solution (1,000 mg/L or 100 mg/L). for arsenic, cadmium, chromium
and lead, adopt single-element or multi-element standard stock solutions certified by the state
and awarded a reference material certificate. It shall remain valid for 1 year.
3.3.2 Internal standard element solution (1,000 mg/L or 100 mg/L). for scandium, germanium,
rhodium, indium, rhenium and bismuth, adopt single-element or multi-element standard stock
solutions certified by the state and awarded a reference material certificate. It shall remain valid
for 2 years.
3.4 Preparation of Standard Solutions
3.4.1 Mixed standard working solution. accurately draw an appropriate amount of single-
element or multi-element mixed standard stock solution, use nitric acid solution (5 + 95) to
dilute it step by step to prepare a mixed standard series solution. The concentration of each
element is shown in Table A.1 in Appendix A. After the mixed standard series solution is
prepared, transfer it to a brown glass container and store it away from light at room temperature.
It shall remain valid for 1 month.
NOTE. the concentration and range of the element in the standard series solution can be
appropriately adjusted in accordance with the sensitivity and linear range of the instrument,
and the actual content of each element in the specimen solution.
4 Instruments and Equipment
NOTE. all glassware and plasticware need to be soaked in nitric acid solution (1 + 4) overnight,
rinsed with water and reserved for later use.
4.1 Inductively coupled plasma mass spectrometer (ICP-MS).
4.2 Analytical balance. with a division value of 0.1 mg.
4.3 Microwave digestion instrument. equipped with a polytetrafluoroethylene digestion inner
tank.
4.4 Pressure digestion tank. equipped with a polytetrafluoroethylene digestion inner tank.
4.5 Temperature-controllable electric hot plate.
5 Analytical Procedures
5.1 Specimen Preparation
Take an appropriate amount of sample, use an appropriate crushing equipment to cut or grind
the sample into powder, and evenly mix it.
5.2 Specimen Digestion
5.2.1 Microwave digestion method
5.2.2 Pressure tank digestion method
5.2.2.1 Preparation of specimen solution
Weigh-take 0.5 g (accurate to 0.1 mg) of the crushed specimen, place it in the
polytetrafluoroethylene digestion inner tank, add 5 mL ~ 8 mL of nitric acid, cover it and leave
it for 1 h. Seal the digestion inner tank in the stainless-steel outer tank, and place it in a constant-
temperature drying oven for digestion (see Table B.1 in Appendix B for the reference conditions
of digestion). After digestion, wait until the digestion tank has been completely cooled down
before slowly opening the inner cover. Use a small amount of water to rinse the inner cover
twice and put it in the digestion tank. Place the digestion tank on the temperature-controllable
electric hot plate and heat it at about 140 C for 30 min, or place it in the ultrasonic cleaning
machine for 5 min. Transfer all the digestion solution to a 25 mL or 50 mL volumetric flask,
use water to reach a constant volume to the scale, evenly mix it and reserve it for later testing.
5.2.2.2 Blank test
Except that no specimen is added, proceed in accordance with 5.2.2.1 to obtain a blank test
solution.
5.3 Reference Conditions of Instrument
5.3.1 Instrument operating conditions
The reference working conditions of the instrument are shown in Table B.2 in Appendix B. The
element reference analysis mode is shown in Table B.3 in Appendix B.
NOTE. for instruments that do not have a suitable interference elimination mode, it is necessary to
adopt the interference correction equations to correct the determination results. The
interference correction equation for arsenic, cadmium and lead, etc. are shown in Table B.4
in Appendix B.
6 Expression of Analysis Results
The residual amount of the element to be determined in the specimen is calculated in accordance
with Formula (1).
7 Precision
When the residual amount of each element in food contact materials and products is > 1.00
mg/kg, the absolute difference between the results of two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean. When 0.100 mg/kg
< the residual amount of each element 1.00 mg/kg, the absolute difference between the results
of two independent determinations obtained under repeatability conditions shall not exceed 15%
of the arithmetic mean. When the residual amount of each element is 0.100 mg/kg, the
absolute difference between the results of two independent determinations obtained under
repeatability conditions shall not exceed 20% of the arithmetic mean.
8 Others
When the sampling size is 0.5 g and the constant volume is 50 mL, the detection limit and
quantitation limit of each element are shown in Table 1.
9 Principle
After the specimen is crushed, use nitric acid for digestion. After the obtained solution is diluted
with water to a constant volume, adopt an inductively coupled plasma optical emission
spectrometer to conduct the determination. Take the wavelength of the element’s characteristic
spectral line for qualitative analysis and the external standard method for quantitative analysis.
Element
10.1 Reagents
10.1.1 Nitric acid (HNO3). excellent-grade pure or higher.
10.1.2 Argon (Ar). argon ( 99.995%) or liquid argon.
10.2 Preparation of Reagents
10.2.1 Nitric acid solution (5 + 95). measure-take 50 mL of nitric acid, slowly add it to 950 mL
of water and evenly mix it.
10.2.2 Nitric acid solution (1 + 4). measure-take 1 L of nitric acid, slowly add it to 4 L of water
and evenly mix it.
10.3 Reference Materials
Element standard solution (1,000 mg/L or 100 mg/L). for arsenic, cadmium, chromium and
lead, adopt single-element or multi-element standard stock solutions certified by the state and
awarded a reference material certificate. It shall remain valid for 1 year.
11 Instruments and Equipment
NOTE. all glassware and plasticware need to be soaked in nitric acid solution (1 + 4) overnight,
rinsed with water and reserved for later use.
11.1 Inductively coupled plasma optical emission spectrometer (ICP-OES).
11.2 Balance. with a division value of 0.1 mg.
11.3 Microwave digestion instrument. equipped with a polytetrafluoroethylene digestion inner
tank.
11.4 Pressure digestion tank. equipped with a polytetrafluoroethylene digestion inner tank.
12 Analytical Procedures
12.1 Specimen Preparation
Same as 5.1.
12.2 Specimen Digestion
12.2.1 Microwave digestion method
Same as 5.2.1.
12.2.2 Pressure tank digestion method
Same as 5.2.2.
12.3 Reference Conditions of Instrument
Optimize the working conditions, so that the indicators, for example, sensitivity, of the elements
to be determined reach the analysis requirements. Edit the determination method and select the
appropriate analytical spectral line for each element to be determined. The reference conditions
of instrument operation are shown in B.3.1 in Appendix B. The recommended analytical
spectral lines of the elements to be determined are shown in Table B.6 in Appendix B.
12.4 Drawing of Standard Curve
Inject the mixed standard working solution into the inductively coupled plasma optimal
emission spectrometer. In accordance with the concentration from low to high, determine the
signal response values of the intensity of the analytical spectral lines of the elements to be
determined. Take the concentration of the element to be determined as the x-coordinate, and the
intensity response value of its analytical spectral line as the y-coordinate to draw a standard
curve.
13 Expression of Analysis Results
The residual amount of the element to be determined in the specimen is calculated in accordance
with Formula (2).
14 Precision
Same as Chapter 7.
15 Others
When the sampling size is 0.5 g and the constant volume is 50 mL, the detection limit and
quantitation limit of each element are shown in Table 2.
16 Principle
After the migration test is conducted on the food contact materials and products, conduct pre-
treatment of the soaking solution, and adopt an inductively coupled plasma mass spectrometer
to conduct the determination. Take the specific mass number of the element (mass-to-charge
ratio, m/z) for qualitative analysis and the external standard method for quantitative analysis.
17 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all excellent-grade pure,
and the water is Grade-1 water specified in GB/T 6682.
17.1 Reagents
17.1.1 Nitric acid (HNO3). excellent-grade pure or higher.
17.1.2 Argon (Ar). argon ( 99.995%) or liquid argon.
17.1.3 Helium (He). helium ( 99.995%).
17.1.4 Reagents required for the preparation of food simulants. in accordance with the
stipulations of GB 5009.156.
17.2 Preparation of Reagents
Detection
17.3 Reference Materials
17.3.1 Element standard solution (1,000 mg/L or 100 mg/L). for aluminum, arsenic, barium,
cadmium, cobalt, chromium, copper, iron, lithium, manganese, molybdenum, nickel, lead,
antimony, tin and zinc, adopt single-element or multi-element standard stock solutions certified
by the state and awarded a reference material certificate. It shall remain valid for 1 year.
17.3.2 Internal standard element solution (1,000 mg/L or 100 mg/L). for scandium, germanium,
rhodium, indium, rhenium and bismuth, adopt single-element or multi-element standard stock
solutions certified by the state and awarded a reference material certificate. It shall remain valid
for 2 years.
17.4 Preparation of Standard Solutions
17.4.1 Mixed standard working solution. accurately draw an appropriate amount of single-
element or multi-element mixed standard stock solution, use 4% (volume fraction) acetic acid
solution [applicable to 4% (volume fraction) acetic acid specimen solution], 1 g/L citric acid
solution and 5 g/L citric acid solution (respectively applicable to citric acid specimen solutions
of different concentrations), nitric acid solution (5 + 95) (applicable to artificial tap water,
alcohol, isooctane and olive oil specimen solutions) to dilute it step by step to prepare a mixed
standard series solution. The concentration of each element is shown in Table A.3 in Appendix
A. After the mixed standard series solution is prepared, transfer it to a brown glass container
and store it at room temperature. It shall remain valid for 1 month.
NOTE. the concentration and range of the element in the standard series solution can be
appropriately adjusted in accordance with the sensitivity and linear range of the instrument,
and the actual content of each element in the food simulant migration specimen solution.
17.4.2 Internal standard working solution. take an appropriate amount of internal standard
single-element stock solution or internal standard multi-element stock solution, use nitric acid
solution (5 + 95) to prepare a multi-element internal standard used solution of an appropriate
concentration. After the specimen solution is mixed, the reference concentrations of the internal
standard elements are shown in A.5 in Appendix A. After the internal standard working solution
is prepared, transfer it to a brown glass container and store it at room temperature. It shall
remain valid for 1 month.
18 Instruments and Equipment
NOTE. all glassware and plasticware need to be soaked in nitric acid solution (1 + 4) overnight,
rinsed with water and reserved for later use.
18.1 Inductively coupled plasma mass spectrometer (ICP-MS).
18.2 Analytical balance. with a division value of 0.01 g and 0.1 mg, respectively.
18.3 Temperature-controllable electric hot plate.
18.4 Rotary evaporator.
18.5 Microporous filter membrane. hydrophilic PTFE, 0.45 m.
19 Analytical Procedures
19.1 Specimen Preparation
19.1.1 Types of food simulants
In this Standard, the migration test adopts 4% (volume fraction) acetic acid, 10% (volume
fraction) ethanol, 20% (volume fraction) ethanol, 50% (volume fraction) ethanol, 95% (volume
fraction) ethanol, 1 g/L citric acid, 5 g/L citric acid, artificial tap water, olive oil and isooctane
as food simulants.
19.1.2 Migration test
In accordance with the intended purposes and usage conditions of the sample to be tested, and
the migration test methods and test conditions specified in GB 5009.156, GB 31604.1 and the
stipulations of relevant product standards, conduct the migration test. After the food simulant
soaking solution is thoroughly mixed, take part of the soaking solution for analysis.
19.1.3 Preparation of specimen solution
19.1.3.1 4% (volume fraction) acetic acid and citric acid specimen solution
Filter 4% (volume fraction) acetic acid soaking solution, 1 g/L citric acid and 5 g/L citric acid
soaking solution through the microporous filter membrane, then, directly inject it for
determination.
19.1.3.2 Artificial tap water specimen solution
Take 2.5 mL of nitric acid and place it in a 50 mL volumetric flask. Use the filtrate of the
artificial tap water soaking solution filtered through the microporous filter membrane to reach
a constant volume, evenly mix it and reserve it for later use.
19.1.3.3 Alcohol specimen solution
Accurately weigh-take 10 g (accurate to 0.01 g) of 10% (volume fraction) ethanol, 20% (volume
fraction) ethanol, 50% (volume fraction) ethanol and 95% (volume fraction) ethanol soaking
solution into a digestion tube or 100 mL conical flask. Place it on a temperature-controllable
electric hot plate, at about 150 C, evaporate the specimen solution to almost dryness, then, add
5 mL of nitric acid solution (5 + 95), continue heating for 5 min ~ 10 min and prevent
evaporation to dryness. Take it out and cool to room temperature, then, use nitric acid solution
(5 + 95) to transfer and reach a constant volume of 10 mL, evenly mix it and reserve it for later
use.
21 Precision
When the content of each element in food simulant specimen solution is > 1.00 mg/kg, the
absolute difference between the results of two independent determinations obtained under
repeatability conditions shall not exceed 10% of the arithmetic mean. When 0.100 mg/kg < the
content of each element 1.00 mg/kg, the absolute difference between the results of two
independent determinations obtained under repeatability conditions shall not exceed 15% of the
arithmetic mean. When the content of each element is 0.100 mg/kg, the absolute difference
between the results of two independent determinations obtained under repeatability conditions
shall not exceed 20% of the arithmetic mean.
22 Others
When the sampling size is 0.5 g and the constant volume is 25 mL, the detection limit and
quantitation limit of each element in olive oil food simulant are shown in Table 3; the detection
limit and quantitative limit of each element in other food simulants are shown in Table 4.
23 Principle
After the migration test is conducted on the food contact materials and products, conduct pre-
treatment of the soaking solution, and adopt an inductively coupled plasma optical emission
spectrometer to conduct the determination. Take the wavelength of the element’s characteristic
spectral line for qualitative analysis and the external standard method for quantitative analysis.
No. Detection Limit mg/kg
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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