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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
GB 31604.49-2023
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
11 Instruments and Equipment ... 11
12 Analytical Procedures ... 12
13 Expression of Analysis Results ... 13
14 Precision ... 13
15 Others ... 13
Part 2 - Determination of Aluminum, Arsenic, Barium, Cadmium, Cobalt, Chromium,
Copper, Iron, Lithium, Manganese, Molybdenum, Nickel, Lead, Antimony, Tin and
Zinc Migration ... 14
Method 1 Inductively Coupled Plasma Mass Spectrometry ... 14
16 Principle ... 14
17 Reagents and Materials ... 14
18 Instruments and Equipment ... 16
19 Analytical Procedures ... 16
20 Expression of Analysis Results ... 18
21 Precision ... 19
22 Others ... 19
Method 2 Inductively Coupled Plasma Optical Emission Spectrometry ... 20
23 Principle ... 20
24 Reagents and Materials ... 21
25 Instruments and Equipment ... 22
26 Analytical Procedures ... 22
27 Expression of Analysis Results ... 23
28 Precision ... 24
29 Others ... 24
Appendix A Mass Concentration of Standard Series Solution ... 25
Appendix B Reference Conditions of Instrument ... 28
National Food Safety Standard - Food Contact Materials
and Products - Determination of Multi-elements and
Determination of Multi-element Migration
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.
3.4.2 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 working 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 away from light at room
tank out of the digestion instrument. After the digestion tank has been completely cooled down,
slowly open 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.
5.2.1.2 Blank test
Except that no specimen is added, proceed in accordance with 5.2.1.1 to obtain a blank test
solution.
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.
5.3.2 Reference conditions of determination
Under the operating conditions of the selected instrument, edit the determination method; in
accordance with the properties of the element to be determined, select the corresponding
10 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.
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.
10.4 Preparation of Standard Solution
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 mass concentration of each element is
shown in Table A.2 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.
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.
17.2.1 Food simulant: 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 and artificial tap water, which are prepared in accordance with
the stipulations of GB 5009.156.
17.2.2 Nitric acid solution (5 + 95): measure-take 50 mL of nitric acid, slowly add it to 950 mL
of water and evenly mix it.
17.2.3 Nitric acid solution (1 + 4): measure-take 1 L of nitric acid, slowly add it to 4 L of water
and evenly mix it.
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.
NOTE: the internal standard solution can be manually and quantitatively added when preparing the
mixed standard series solution and the specimen solution to be tested, or it can be added
online by the instrument. The internal standard concentrati...