Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces the determination of arsenic and migration in GB/T 5009.68-2003 Method for Analysis of Hygienic Standard of Perchlorovinyl-coating for Inner Wall of Food Container, GB/T 5009.72-2003 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, SN/T 2900-2011 Food Contact Materials for Export. Paper, Regenerated Fibre Materials. Determination of Arsenic. Hydride Generation-atomic Fluorescence Spectrometry, SN/T 2594-2010 Food Contact Materials - Determination of Lead, Cadmium, Chromium, and Arsenic In Cork Stoppers By Inductively Coupled Plasma Mass Spectrometry, 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 2829-2011 Food Contact Materials For Export-Metal Materials-Determination of Migrant Heavy Metals in Food Simulant-inductively Coupled Plasma Atomic Emission Spectrometric Method.
The following main changes have been made with respect to GB/T 5009.68-2003 (the previous edition):
——The name of this standard is revised as National Food Safety Standard - Food Contact Materials and Articles - Determination of Arsenic and Migration;
——Determination of arsenic is added;
——Inductively coupled plasma mass spectrometry is added;
——Inductively coupled plasma atomic emission spectrometry is added;
——Silver salt method and arsenic stain method are deleted.
National Food Safety Standard
Food Contact Materials and Articles-
Determination of Arsenic and Migration
1 Scope
This standard specifies hydride-atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry and inductively coupled plasma emission spectrometry for the determination of arsenic migration in food contact materials and articles after being soaked in food simulants and also the determination of arsenic in paper product and cork.
This standard is applicable to the determination of arsenic migration in food contact materials and articles and arsenic in paper product and cork.
Part I Determination of Arsenic
Method I Hydride-atomic Fluorescence Spectrometry
2 Principle
Digest the paper product and cork with dry ashing after grinding, add sulfourea into digestion solution to pre-reduce the pentavalent arsenic into trivalent arsenic, generate arsenic hydride with reduced hydrogen, carry it by argon to quartz atomizer to be decomposed into atomic arsenic, and generate atomic fluorescence under excitation of emitting light from arsenic hollow cathode lamp. Its fluorescence intensity is in direct proportional to the arsenic concentration in tested liquid and compare with standard series for quantification.
3 Reagents and Materials
Unless otherwise specified, analytically-pure reagents and Class-II water (defined in GB/T 6682) are adopted for the purpose of this method.
3.2.1 Potassium hydroxide solution(5g/L): weigh 5g potassium hydroxide, dilute with water to 1000mL, then mix uniformly.
3.2.2 Potassium borohydride alkali solution (10g/L): weigh 10g potassium borohydride, dissolve with potassium hydroxide solution (5g/L) and scale the volume to 1000mL. Such solution is prepared immediately before use.
3.2.3 Pre-reducing agent solution: weigh 5.0g sulfourea, dissolve with about 80mL water, add 5.0g ascorbic acid, dilute with water to 100mL after fully dissolving, and then mix uniformly; it is prepared immediately before use.
3.2.4 Hydrochloric acid solution(5+95): measure 50mL hydrochloric acid and pour it into 950mL water, and mix uniformly.
3.2.5 Hydrochloric acid solution(1+1): measure 50mL hydrochloric acid and pour it into 50mL water, and mix uniformly.
3.2.6 Magnesium nitrate solution(150g/L): weigh 16.13g magnesium nitrate hexahydrate, dilute with water to 100mL, then mix uniformly.
3.3 Standard product
Arsenic trioxide (As2O3, CAS No.: 1327-53-3): with purity>99.99%, or arsenic standard solution in certain concentration approved and awarded with reference material certificate by the State.
3.4 Preparation of standard solutions
3.4.1 Arsenic standard stock solution (1000mg/L): prepare with the standard solution approved and awarded with reference material certificate by the State or according to the requirements of GB/T 602.
3.4.2 Arsenic standard intermediate solution(1.00mg/L): accurately pipet 10.0mL arsenic standard stock solution to a 100mL volumetric flask, add hydrochloric acid solution (5+95) to the scale, and mix uniformly. Accurately pipet 1.00mL such arsenic standard solution again into 100mL volumetric flask, add hydrochloric acid solution (5+95) to the scale and mix uniformly.
3.4.3 Arsenic standard series solutions: respectively pipet 0mL, 0.500mL, 1.00mL, 2.00mL, 3.00mL and 4.00mL arsenic standard intermediate solution into 100mL volumetric flasks, add hydrochloric acid solution (5+95) to the scale and mix uniformly. The concentrations of such arsenic standard series solutions are 0μg/L, 5.00μg/L, 10.0μg/L, 20.0μg/L, 30.0μg/L and 40.0μg/L respectively.
Note: the specific concentration of arsenic in standard solution series may be determined according to the sensitivity of instrument, linear range and the actual arsenic concentration in the soak solution.
4 Instruments and Apparatus
Note: all glassware shall be soaked in nitric acid (1+5) overnight, flushed with tap water repeatedly, and finally washed clean with water.
4.1 Atomic fluorescence spectrophotometer: with arsenic hollow cathode lamp.
4.2 Muffle furnace.
4.3 Analytical balance: with sensibility of 1mg.
5 Analysis Steps
5.1 Pretreatment of specimen
Take appropriate specimen and mix uniformly after grinding. Weigh 1~3g (accurate to 0.001g) specimen and put into a crucible with cover, add 10mL magnesium nitrate solution (150g/L), mix uniformly, evaporate to dryness under low heat, cover 1g magnesium oxide on dry slag carefully, carbonize on electric furnace till there is no black smoke, and transfer into 550℃ high temperature furnace to ash for 4h. Take it out, cool, add 10mL hydrochloric acid solution (1+1) to neutralize magnesium oxide carefully and dissolve ash content, transfer into a 25mL volumetric flask, transfer and put into volumetric flask after rinsing the crucible with hydrochloric acid solution (5+95) for several times, and finally dilute with water to the scale and mix uniformly for standby.
5.2 Determination
5.2.1 Test conditions of instruments
Regulate the instrument performance to optimum condition, and the reference conditions of instruments: voltage of photomultiplier: 400V; current of arsenic hollow cathode lamp: 35mA; atomizer: temperature: 820~850℃; height: 8mm; flow rate of argon: carrier gas 400mL/min.
5.2.2 Plotting of standard curve
Take 6 pieces of 25mL colorimetric cylinders, accurately add 20mL arsenic standard series solutions successively, add 5mL prereducing agent solution respectively, mix uniformly and test after placing for 30min. Lead the standard series solutions into atomic fluorescence spectrophotometer from low concentration to high concentration, determine the fluorescence intensity and plot the standard curve with the concentration as x-axis and the absorbance value as y-axis.
5.2.3 Determination of specimen
Put 20mL specimen digestion solution into a 25mL colorimetric cylinder, add 5mL prereducing agent solution, mix uniformly, determine after placing for 30min, compare with standard series for quantification and carry out blank test simultaneously.
6 Expression of Analysis Results
The arsenic content in the specimen is calculated according to Formula (1):
(1)
Where,
X——the arsenic content in the specimen, mg/kg;
ρ——the arsenic concentration in determined specimen digestion solution, μg/L;
ρ0——the arsenic concentration in blank solution, μg/L;
V——the total constant volume of specimen digestion solution, mL;
m——the mass of specimen, g;
1000——the conversion coefficient.
Where the arsenic content ≥1.00mg/kg, three significant figures shall be reserved for the calculation results; where the arsenic content <1.00mg/kg, two significant figures shall be reserved for the calculation results.
7 Accuracy
The absolute difference of the results from two independent determinations under repeatability condition shall not exceed 20% of their arithmetic average.
Foreword i 1 Scope 2 Principle 3 Reagents and Materials 4 Instruments and Apparatus 5 Analysis Steps 6 Expression of Analysis Results 7 Accuracy 8 Other 9 Principle 10 Reagents and Materials 11 Instruments and Apparatus 12 Analysis Steps 13 Expression of Analysis Results 14 Accuracy 15 Other
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces the determination of arsenic and migration in GB/T 5009.68-2003 Method for Analysis of Hygienic Standard of Perchlorovinyl-coating for Inner Wall of Food Container, GB/T 5009.72-2003 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, SN/T 2900-2011 Food Contact Materials for Export. Paper, Regenerated Fibre Materials. Determination of Arsenic. Hydride Generation-atomic Fluorescence Spectrometry, SN/T 2594-2010 Food Contact Materials - Determination of Lead, Cadmium, Chromium, and Arsenic In Cork Stoppers By Inductively Coupled Plasma Mass Spectrometry, 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 2829-2011 Food Contact Materials For Export-Metal Materials-Determination of Migrant Heavy Metals in Food Simulant-inductively Coupled Plasma Atomic Emission Spectrometric Method.
The following main changes have been made with respect to GB/T 5009.68-2003 (the previous edition):
——The name of this standard is revised as National Food Safety Standard - Food Contact Materials and Articles - Determination of Arsenic and Migration;
——Determination of arsenic is added;
——Inductively coupled plasma mass spectrometry is added;
——Inductively coupled plasma atomic emission spectrometry is added;
——Silver salt method and arsenic stain method are deleted.
National Food Safety Standard
Food Contact Materials and Articles-
Determination of Arsenic and Migration
1 Scope
This standard specifies hydride-atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry and inductively coupled plasma emission spectrometry for the determination of arsenic migration in food contact materials and articles after being soaked in food simulants and also the determination of arsenic in paper product and cork.
This standard is applicable to the determination of arsenic migration in food contact materials and articles and arsenic in paper product and cork.
Part I Determination of Arsenic
Method I Hydride-atomic Fluorescence Spectrometry
2 Principle
Digest the paper product and cork with dry ashing after grinding, add sulfourea into digestion solution to pre-reduce the pentavalent arsenic into trivalent arsenic, generate arsenic hydride with reduced hydrogen, carry it by argon to quartz atomizer to be decomposed into atomic arsenic, and generate atomic fluorescence under excitation of emitting light from arsenic hollow cathode lamp. Its fluorescence intensity is in direct proportional to the arsenic concentration in tested liquid and compare with standard series for quantification.
3 Reagents and Materials
Unless otherwise specified, analytically-pure reagents and Class-II water (defined in GB/T 6682) are adopted for the purpose of this method.
3.1 Reagents
3.1.1 Potassium hydroxide (KOH).
3.1.2 Potassium borohydride (KBH4).
3.1.3 Sulfourea (CN2H4S).
3.1.4 Ascorbic acid (C6H8O6).
3.1.5 Nitric acid (HNO3): guaranteed reagent.
3.1.6 Hydrochloric acid (HCl): guaranteed reagent.
3.1.7 Magnesium nitrate hexahydrate [Mg(NO3)2·6H2O].
3.1.8 Magnesium oxide (MgO).
3.2 Preparation of reagents
3.2.1 Potassium hydroxide solution(5g/L): weigh 5g potassium hydroxide, dilute with water to 1000mL, then mix uniformly.
3.2.2 Potassium borohydride alkali solution (10g/L): weigh 10g potassium borohydride, dissolve with potassium hydroxide solution (5g/L) and scale the volume to 1000mL. Such solution is prepared immediately before use.
3.2.3 Pre-reducing agent solution: weigh 5.0g sulfourea, dissolve with about 80mL water, add 5.0g ascorbic acid, dilute with water to 100mL after fully dissolving, and then mix uniformly; it is prepared immediately before use.
3.2.4 Hydrochloric acid solution(5+95): measure 50mL hydrochloric acid and pour it into 950mL water, and mix uniformly.
3.2.5 Hydrochloric acid solution(1+1): measure 50mL hydrochloric acid and pour it into 50mL water, and mix uniformly.
3.2.6 Magnesium nitrate solution(150g/L): weigh 16.13g magnesium nitrate hexahydrate, dilute with water to 100mL, then mix uniformly.
3.3 Standard product
Arsenic trioxide (As2O3, CAS No.: 1327-53-3): with purity>99.99%, or arsenic standard solution in certain concentration approved and awarded with reference material certificate by the State.
3.4 Preparation of standard solutions
3.4.1 Arsenic standard stock solution (1000mg/L): prepare with the standard solution approved and awarded with reference material certificate by the State or according to the requirements of GB/T 602.
3.4.2 Arsenic standard intermediate solution(1.00mg/L): accurately pipet 10.0mL arsenic standard stock solution to a 100mL volumetric flask, add hydrochloric acid solution (5+95) to the scale, and mix uniformly. Accurately pipet 1.00mL such arsenic standard solution again into 100mL volumetric flask, add hydrochloric acid solution (5+95) to the scale and mix uniformly.
3.4.3 Arsenic standard series solutions: respectively pipet 0mL, 0.500mL, 1.00mL, 2.00mL, 3.00mL and 4.00mL arsenic standard intermediate solution into 100mL volumetric flasks, add hydrochloric acid solution (5+95) to the scale and mix uniformly. The concentrations of such arsenic standard series solutions are 0μg/L, 5.00μg/L, 10.0μg/L, 20.0μg/L, 30.0μg/L and 40.0μg/L respectively.
Note: the specific concentration of arsenic in standard solution series may be determined according to the sensitivity of instrument, linear range and the actual arsenic concentration in the soak solution.
4 Instruments and Apparatus
Note: all glassware shall be soaked in nitric acid (1+5) overnight, flushed with tap water repeatedly, and finally washed clean with water.
4.1 Atomic fluorescence spectrophotometer: with arsenic hollow cathode lamp.
4.2 Muffle furnace.
4.3 Analytical balance: with sensibility of 1mg.
5 Analysis Steps
5.1 Pretreatment of specimen
Take appropriate specimen and mix uniformly after grinding. Weigh 1~3g (accurate to 0.001g) specimen and put into a crucible with cover, add 10mL magnesium nitrate solution (150g/L), mix uniformly, evaporate to dryness under low heat, cover 1g magnesium oxide on dry slag carefully, carbonize on electric furnace till there is no black smoke, and transfer into 550℃ high temperature furnace to ash for 4h. Take it out, cool, add 10mL hydrochloric acid solution (1+1) to neutralize magnesium oxide carefully and dissolve ash content, transfer into a 25mL volumetric flask, transfer and put into volumetric flask after rinsing the crucible with hydrochloric acid solution (5+95) for several times, and finally dilute with water to the scale and mix uniformly for standby.
5.2 Determination
5.2.1 Test conditions of instruments
Regulate the instrument performance to optimum condition, and the reference conditions of instruments: voltage of photomultiplier: 400V; current of arsenic hollow cathode lamp: 35mA; atomizer: temperature: 820~850℃; height: 8mm; flow rate of argon: carrier gas 400mL/min.
5.2.2 Plotting of standard curve
Take 6 pieces of 25mL colorimetric cylinders, accurately add 20mL arsenic standard series solutions successively, add 5mL prereducing agent solution respectively, mix uniformly and test after placing for 30min. Lead the standard series solutions into atomic fluorescence spectrophotometer from low concentration to high concentration, determine the fluorescence intensity and plot the standard curve with the concentration as x-axis and the absorbance value as y-axis.
5.2.3 Determination of specimen
Put 20mL specimen digestion solution into a 25mL colorimetric cylinder, add 5mL prereducing agent solution, mix uniformly, determine after placing for 30min, compare with standard series for quantification and carry out blank test simultaneously.
6 Expression of Analysis Results
The arsenic content in the specimen is calculated according to Formula (1):
(1)
Where,
X——the arsenic content in the specimen, mg/kg;
ρ——the arsenic concentration in determined specimen digestion solution, μg/L;
ρ0——the arsenic concentration in blank solution, μg/L;
V——the total constant volume of specimen digestion solution, mL;
m——the mass of specimen, g;
1000——the conversion coefficient.
Where the arsenic content ≥1.00mg/kg, three significant figures shall be reserved for the calculation results; where the arsenic content <1.00mg/kg, two significant figures shall be reserved for the calculation results.
7 Accuracy
The absolute difference of the results from two independent determinations under repeatability condition shall not exceed 20% of their arithmetic average.
Contents of GB 31604.38-2016
Foreword i
1 Scope
2 Principle
3 Reagents and Materials
4 Instruments and Apparatus
5 Analysis Steps
6 Expression of Analysis Results
7 Accuracy
8 Other
9 Principle
10 Reagents and Materials
11 Instruments and Apparatus
12 Analysis Steps
13 Expression of Analysis Results
14 Accuracy
15 Other
