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GB 31604.34-2016 PDF English

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GB 31604.34-2016: National food safety standard - Food Contact Materials and Products - Determination of Lead and Its Migration
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GB 31604.34-2016: National food safety standard - Food Contact Materials and Products - Determination of Lead and Its 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 Lead and Its 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... 4 1 Application Scope... 5 Part I – Determination of Lead... 5 2 Principle... 5 3 Reagents and Materials... 5 4 Apparatus... 6 5 Analytical Procedure... 7 6 Expression of Analytical Results... 7 7 Accuracy... 8 8 Others... 8 Part II – Determination of Lead Migration... 8 9 Principle... 8 10 Reagents and Materials... 9 11 Apparatus... 10 12 Analytical Procedure... 10 13 Expression of Analytical Results... 11 14 Accuracy... 11 15 Others... 11 16 Principle... 11 17 Reagents and Materials... 12 18 Apparatus... 13 19 Analytical Procedure... 13 20 Expression of Analytical Results... 13 21 Accuracy... 14 22 Others... 14 Annex A Reference Temperature Rise Procedure for Graphite Furnace Atomic Absorption Spectrometer... 15 Annex B Reference Operating Conditions for Flame Atomic Absorption Spectrometer... 16

Foreword

This Standard replaces the determination of lead of its migration of GB/T 5009.62- 2003, Method for analysis of hygienic standard of ceramics for food containers, GB/T 5009.63-2003, Method for analysis of hygienic standard of enamel for food containers, GB/T 5009.72, Method for analysis of hygienic standard of aluminum-wares for food use, GB/T 5009.78-2003, Method for analysis of hygienic standard of papers for food packaging, GB/T 5009.81-2003, Method for analysis of hygienic standard of stainless steel food containers and table wares, GB/T 3534-2002, Standard testing methods for lead and cadmium release from domestic ceramics, GB 8058-2003, Standard permissible limits and testing method for release of lead or cadmium from ceramic cookware, GB/T 21170-2007, Glass hollowware – Test method for lead and cadmium release, 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, 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 2886, Food contact materials for export – Determination of lead and cadmium release in glass container simulants, and SN/T 2594-2010, Food contact materials – Determination of lead, cadmium, chromium, and arsenic in cork stoppers by inductively coupled plasma mass spectrometry. Compared with GB/T 5009.62-2003, the main changes of this Standard are as follows. -- it changes the name of the standard into “National Food Safety Standard – Food Contact Materials and Products – Determination of Lead and Its Migration”; -- it adds the determination of lead; -- it adds the graphite furnace atomic absorption spectrometric method; -- it adds the inductively coupled plasma mass spectrometric method; -- it adds the inductively coupled plasma atomic emission spectrometric method; and -- it deletes the dithizone colorimetric method. National Food Safety Standard – Food Contact Materials and Products – Determination of Lead and Its Migration

1 Application Scope

This Standard specifies the graphite furnace atomic absorption spectrometric method, inductively coupled plasma mass spectrometric method, inductively coupled plasma atomic emission spectrometric method and flame atomic absorption spectrometric method for the determination of lead in paper products and cork stoppers and lead migration after being soaked in the food simulants. This Standard applies to the determination of lead in paper products and cork stoppers and lead migration in food contact materials and products. Part I – Determination of Lead Method I – Graphite Furnace Atomic Absorption Spectrometric Method

2 Principle

Grind the paper products or cork stoppers; use the dry method for digestion; atomize the digestion solution in a graphite furnace; determine absorbency by comparing with the standard series (the absorption value measured at 283.3 nm within a certain concentration range is in direct proportion to the lead content).

3 Reagents and Materials

Unless specified otherwise, all reagents used for this method are guaranteed reagents and the water is water grade II specified in GB/T 6682. 3.1 Reagents 3.2 Preparation of reagents 3.2.1 Nitric acid solution (5 + 95). measure 50 mL of nitric acid; add to 950 L of water; and mix up. 3.2.2 Nitric acid solution (1 + 9). measure 50 mL of nitric acid; add to 450 L of water; and mix up. 3.3 Standard substance Lead nitrate [Pb(NO3)2, CAS no.. 10099-74-8]. purity > 99.99% or the lead standard solution of a certain concentration which has been certified by a national certification institution and awarded the certificate of standard substance. 3.4 Preparation of standard solutions 3.4.1 Lead standard stock solution (1 000 mg/L). weigh accurately 1.598 5 g (accurate to 0.000 1 g); use a small amount of nitric acid solution (1 + 9) to dissolve; transfer to a 1000 mL volumetric flask; add water to scale and mix up.

4 Apparatus

NOTE All glass wares shall be soaked in nitric acid (1 + 5) overnight, washed with tap water repeatedly and washed clean in the end. 4.1 Atomic absorption spectrometer. equipped with graphite furnace atomizer and attached with lead hollow cathode lamp. 4.2 Adjustable electric hot plate.

5 Analytical Procedure

5.1 Digestion of sample Take an appropriate amount of sample, grind and mix up. Weigh 1 g to 5 g (accurate to 0.001 g) of sample to place into a crucible; first use soft fire to carbonize to smokeless on an adjustable electric hot plate; transfer to muffle furnace at 500˚C for ashing for 6 h to 8 h and then cool down. 5.2 Determination 5.2.1 Apparatus testing conditions See Table A.1 for the reference conditions. 5.2.2 Establishment of standard curve In accordance with the sequence of concentrations from low to high, put 10 μL of lead standard serial solution and 5 μL of palladium nitrate solution-ammonium dihydrogen phosphate solution (the sample size can be decided in accordance with the apparatus used) respectively into the graphite furnace at the same time; 5.2.3 Determination of sample Place 10 μL of blank solution or sample solution and 5 μL of palladium nitrate solution- ammonium dihydrogen phosphate solution (the sample size can be decided in accordance with the apparatus used) into a graphite furnace at the same time;

6 Expression of Analytical Results

The lead content in the sample is calculated in accordance with the following equation.

7 Accuracy

The absolute difference between the results obtained from two independent determinations under repeatable conditions shall not exceed 20% of the arithmetic mean value.

8 Others

The calculation is done by weighing 1.0 g of the sample to dilute to 25 mL, with the method detection limit 0.05 mg/kg and quantification limit 0.10 mg/kg.

9 Principle

Use food simulant to soak the intended food contact part of food contact materials and products; use a graphite furnace to atomize the soak solution; determine the absorbance by comparing with the standard series (the absorption value measured at 283.3 nm within a certain concentration range is in direct proportion to the lead content).

10 Reagents and Materials

Unless specified otherwise, all reagents used for this method are guaranteed reagents and the water is water grade II specified in GB/T 6682. 10.1 Reagents 10.1.1 Nitric acid (HNO3). 10.1.2 Ammonium dihydrogen phosphate (NH4H2PO4). 10.1.3 Reagents required for the preparation of food simulant. as specified in GB 10.2 Preparation of reagents 10.2.1 Food simulant. prepared as specified in GB 5009.156. 10.2.2 Nitric acid (5 + 95). measure 50 mL of nitric acid; add to 950 mL of water; and mix up. 10.2.3 Nitric acid (1 + 9). measure 50 mL of nitric acid; add to 450 mL of water; and mix up. 10.2.4 Ammonium dihydrogen phosphate (20 g/L). weigh 2.0 g of ammonium dihydrogen phosphate; use water to dissolve; and dilute to 100 mL. 10.3 Standard substance Lead nitrate [Pb(NO3)2, CAS no.. 10099-74-8]. purity > 99.99% or the lead standard solution of a certain concentration which has been certified by a national certification institution and awarded the certificate of standard substance. 10.4 Preparation of standard solutions 10.4.1 Lead standard stock solution (1 000 mg/L). weigh accurately 1.598 5 g (accurate to 0.000 1 g); use a small amount of nitric acid solution (1 + 9) to dissolve; transfer to a 1000 mL volumetric flask; add water to scale and mix up.

11 Apparatus

NOTE All glass wares shall be soaked in nitric acid (1 + 5) overnight, washed with tap water repeatedly and washed clean in the end. 11.1 Graphite furnace atomic absorption spectrometer. equipped with graphite furnace a ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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