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GB 31604.49-2016 (GB31604.49-2016)

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GB 31604.49-2016
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
National food safety standard –
Food contact materials and articles –
Determination of arsenic, cadmium, chromium
and lead; migration of arsenic, cadmium,
chromium, nickel, lead, antimony and zinc
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by National Health and Family Planning Commission of the PRC
Table of contents
Foreword ... 3 
1 Scope ... 4 
Part I. Determination of arsenic, cadmium, chromium and lead Inductively
coupled plasma mass spectrometry ... 4 
2 Principle... 4 
3 Reagents and materials ... 4 
4 Instruments and equipment ... 6 
5 Analytical procedures ... 6 
6 Expression of analytical results ... 8 
7 Precision... 9 
8 Others ... 9 
Part II. Determination of migration quantity of arsenic, cadmium, chromium,
nickel, lead, antimony, and zinc ... 9 
Method I. Inductively coupled plasma mass spectrometry ... 9 
9 Principle... 9 
10 Reagents and materials... 9 
11 Instruments and equipment ... 11 
12 Analytical procedures ... 11 
13 Expression of analytical results ... 12 
14 Precision ... 13 
15 Others ... 13 
Method II. Inductively coupled plasma - atomic emission spectrometry ... 13 
16 Principle... 13 
17 Reagents and materials... 13 
18 Instruments and equipment ... 14 
19 Analytical procedures ... 15 
20 Expression of analytical results ... 15 
21 Precision ... 15 
22 Others ... 15 
Appendix A Instrument reference working conditions and the recommended
mass-to-charge ratio or analysis wavelength of each element ... 17 
Foreword
This standard replaces the determination of migration quantity of arsenic,
cadmium, chromium, nickel, lead, antimony and zinc as well as the content of
arsenic, cadmium, chromium, and lead in paper products and cork stoppers as
specified in SN/T 2829-2011 “Food contact materials for export - Metal
materials - Determination of migrant heavy metals in food simulant -
Inductively coupled plasma atomic emission spectrometric method”, SN/T
2597-2010 “Determination of lead, cadmium, chromium, arsenic, antimony,
germanium migration quantity in polymer for food contact materials -
Inductively coupled plasma atomic emission spectrometry method”, and SN/T
2594-2010 “Food contact materials - Determination of lead, cadmium,
chromium, and arsenic in cork stoppers by inductively coupled plasma mass
spectrometry”.
As compared with SN/T 2829-2011, SN/T 2597-2010 and SN/T 2594-2010, the
main changes of this standard are as follows.
- CHANGE the standard name into “National food safety standard - Food
contact materials and articles - Determination of arsenic, cadmium,
chromium and lead; migration of arsenic, cadmium, chromium, nickel, lead,
antimony and zinc”.
National food safety standard –
Food contact materials and articles –
Determination of arsenic, cadmium, chromium
and lead; migration of arsenic, cadmium,
chromium, nickel, lead, antimony and zinc
1 Scope
This standard specifies the inductively coupled plasma mass spectrometry and
inductively coupled plasma emission spectrometry for the determination of
arsenic, cadmium, chromium, nickel, lead, antimony and zinc in the food
contact materials and articles after being immersed in food simulants, AND
specifies the inductively coupled plasma mass spectrometry for the
determination of arsenic, cadmium, chromium and lead in paper products and
cork stoppers.
This standard applies to the determination of the migration quantity of arsenic,
cadmium, chromium, nickel, lead, antimony and zinc in various food contact
materials and articles, as well as the determination of arsenic, cadmium,
chromium and lead in paper products and cork stoppers.
Part I. Determination of arsenic, cadmium,
chromium and lead Inductively coupled
plasma mass spectrometry
2 Principle
Paper products and cork stoppers are crushed AND digested by nitric acid;
AND the solution obtained is diluted by water to make its volume reach to the
mark, determined by the inductively coupled plasma mass spectrometry, AND
compared with the standard series for quantitative purposes.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of guarantee
reagent AND the water is level I water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
WEIGH 0.5 g of the crushed sample (accurate to 0.1 mg); PLACE it in the
polytetrafluoroethylene digestion inner tank; ADD 5 mL ~ 8 mL of nitric acid;
COVER it and LET it stand for 1 h; SEAL the digestion tank and PLACE it in
the microwave digestion system; CONDUCT digestion in accordance with the
standard operation procedures of the microwave digestion instrument; AND it
may make reference to the digestion conditions in A.6 for digestion purposes.
After finishing the digestion, TAKE the digestion tank out of the digestion
instrument; when the digestion tank is completely cooled down, slowly OPEN
the inner cover; USE a small amount of water to rinse the inner cover for two
times; COMBINE the rinsing water into the digestion tank. PLACE the
digestion tank onto the temperature control heating plate at 140 °C to heat it for
30 min, or otherwise PLACE it into the ultrasonic water bath ultrasonic for
degassing for 5 min; TRANSFER all the digestion solution into a 50 mL
volumetric flask; USE water to make the volume reach to the mark; MIX it
uniformly; PREPARE for determination. And meanwhile MAKE the sample
blank.
5.2.2 Pressure sealed digestion
WEIGH 0.5 g of the pulverized sample (accurate to 0.1 mg); PLACE it in
polytetrafluoroethylene digestion inner tank; ADD 5 mL ~ 8 mL of nitric acid;
COVER and LET it stand for 1 h; SEAL the digestion inner tank into the
stainless steel outer tank; PLACE it into the constant temperature oven for
digestion; AND it may make reference to the digestion conditions of A.6 for
digestion. After finishing the digestion, when the digestion tank is completely
cooled down, slowly OPEN the inner cover; USE a small amount of water to
rinse the inner cover for two times; COMBINE the rinsing water into the
digestion tank. PLACE the digestion tank onto the temperature control heating
plate at 140 °C to heat it for 30 min, or otherwise PLACE it into the ultrasonic
water bath ultrasonic for degassing for 5 min; TRANSFER all the digestion
solution into a 50 mL volumetric flask; USE water to make the volume reach to
the mark; MIX it uniformly; PREPARE for determination. And meanwhile MAKE
the sample blank.
5.3 Instrument reference conditions
5.3.1 USE the instrument tuning use solution to optimize the working
conditions of the instrument, with the instrument reference conditions as
shown in A.1 AND the element reference analysis mode as shown in A.2.
Note. For instruments that do not have the appropriate interference elimination
mode, it is required to use the interference correction equation to correct the
determination results of arsenic, cadmium and lead. AND the interference
correction equation is as shown in A.3.
5.3.2 In the selected instrument working conditions, EDIT the determination;
SELECT the mass-to-charge ratio of the element to be determined and the
internal standard substance, with the reference conditions as shown in A.1 and
A.2.
10.1.1 Argon (Ar). purity ≥ 99.99%, or liquid argon.
10.1.2 Nitric acid (HNO3).
10.1.3 Helium (He). purity ≥ 99.995%.
10.1.4 Reagents required for preparing food simulant. in accordance with the
provisions of GB 31604.1.
10.2 Reagent preparation
10.2.1 Food simulant. PREPARE it in accordance with the provisions of GB
5009.156.
10.2.2 Nitric acid solution (5 + 95). MEASURE 50 mL of nitric aci...
......
(Above excerpt was released on 2017-06-23, modified on 2021-06-07, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GB31604.49-2016