GB 31604.34-2016 English PDF (GB31604.34-2016)

Delivery: 3 seconds. Download true-PDF + Invoice.
Get Quotation: Click GB 31604.34-2016 (Self-service in 1-minute)
Historical versions (Master-website): GB 31604.34-2016
Preview True-PDF (Reload/Scroll-down if blank)

GB 31604.34-2016: National food safety standard - Food Contact Materials and Products - Determination of Lead and Its Migration
GB 31604.34-2016
Method for analysis of hygienic standard of papers for food packaging
Book People's Republic of China National Standard
National Food Safety Standard
Food contact materials and products
Determination and migration of lead
Published 2016-10-19
2017-04-19 implementation
People's Republic of China
National Health and Family Planning Commission issued
Book GB 31604.34-2016
Foreword
5009.62-2003 "sanitary container standard analytical methods ceramic tableware" Instead of the standard GB/T , GB/T 5009.63-2003
"Enamel for food containers hygienic standard analysis method", GB/T 5009.72-2003 "aluminum food containers and standard analytical methods"
GB/T 5009.78-2003 "food packaging Paper health standard analytical method", GB/T 5009.81-2003 "stainless steel food containers
Hygienic standard analytical method ", GB/T 3534-2002" ceramic ware lead, cadmium release determination ", GB 8058-2003" Ceramic
Cooker lead and cadmium permissible limits and detection methods ", GB/T 21170-2007" glass container lead, cadmium release determination "
SN/T 2597-2010 "food contact materials - Polymer lead, cadmium, chromium, arsenic, antimony, germanium migration Inductively Coupled Plasma
Atomic emission spectrometry ", SN/T 2829-2011" Determination of heavy metals in a metallic material of food contact materials in food simulants
3.4 Standard Preparation
3.4.1 lead standard stock solution (1000mg/L). Accurately weigh 1.5985g (accurate to 0.0001g) lead nitrate, a nitric acid solution with a small amount
(9 + 1) dissolved into 1000mL volumetric flask, add water to volume, and mix.
3.4.2 intermediate lead standard solution (1.00mg/L). a solution of lead draw stock standard solution 1.00mL to 1000mL volumetric flask, add nitric acid
(95 + 5) to volume, and mix.
3.4.3 Standard Series lead solution. Pipette intermediate lead standard solution (1.00mg/L) 0mL, 0.500mL, 1.00mL, 2.00mL, 3.00mL,
4.00mL in 100mL volumetric flask, add a solution of nitric acid (95 + 5) to volume, and mix. This concentration of lead standard solution series, respectively
0μg/L, 5.00μg/L, 10.0μg/L, 20.0μg/L, 30.0μg/L, 40.0μg/L.
Note. The sensitivity of the instrument, the linear range of the sample and the actual content of lead standard solution to determine the concentration of the specific series of lead.
4 instruments and equipment
Note. All glassware required nitric acid solution (1 + 5) soaked overnight, washed repeatedly with water and finally water rinse.
4.1 Atomic absorption spectrometer. graphite furnace atomizer with attached lead hollow cathode lamp.
4.2 adjustable hot plate.
4.3 muffle furnace.
4.4 Analytical balance. a sense of 0.1mg and 1mg.
5 Step analysis
Digestion of samples 5.1
Proper amount of sample was pulverized and mixed. Sample Weigh 1g ~ 5g (accurate to 0.001 g of) in the crucible, a small fire adjustable first heating plate at
Carbonization to smoking, shift 500 ℃ muffle furnace ashing 6h ~ 8h, cooled. If the individual is not completely ashed the sample, then add 1mL adjustable nitrate
Low heat on a hot plate type, repeated several times until the digestion was complete, allowed to cool, with a solution of nitric acid (1 + 1) The ash was dissolved, and transferred into 25mL
Flask, a small amount of water and washed several times crucible and washings were combined in a volumetric flask to volume and mix standby. At the same time as the reagent blank.
5.2 Determination
5.2.1 Instrument Test Conditions
Reference conditions shown in Table A. 1.
5.2.2 standard curve prepared
Sequence from low to high concentration by the standard series 10μL solution of lead nitrate and palladium 5μL - monoammonium phosphate solution (the optimum injection volume can be determined according to the instrument used) simultaneously injected graphite furnace, the measured absorbance atomization value, the concentration of abscissa, the absorbance value of the vertical
Coordinates, the standard curve.
5.2.3 Determination of sample
The 10μL sample solution and a blank solution 5μL or palladium nitrate - monoammonium phosphate solution (the optimum injection volume can be determined according to the instrument used) simultaneously injected graphite furnace, the absorbance value measured for atomization, compared with standard series quantitative .
6 expression analysis results
Lead content in the samples according to the formula (1).
Where.
X---- lead content of the sample, in milligrams per kilogram (mg/kg);
--- [rho] content of lead in a sample solution, in micrograms per liter (μg/L);
--- p0 blank solution lead concentration in micrograms per liter (μg/L); Qiao --- digestive juice sample volume of the total volume in milliliters (mL);
1000 --- conversion factor. When the lead content ≥1.00mg/kg, calculated results to three significant figures, when the lead content < 1.00mg/kg, the results two significant figures.
7 precision
The absolute difference between two measurement results obtained under repeatable conditions not exceed 20% of the arithmetic mean.
8 Other
In sample weight 1.0g, volume to 25mL calculated detection limit was 0.05mg/kg, limit of quantification was 0.10mg/kg.
The second Inductively Coupled Plasma Mass Spectrometry
See GB 31604.49.
The third method of inductively coupled plasma emission spectrometry
See GB 31604.49.
Determination of the second portion of the migration of lead
The first Graphite Furnace Atomic Absorption Spectrometry
Principle 9
Using food simulants and soaking food contact materials in contact with food products contemplated portion soaking solution by graphite furnace atomic, in
The absorbance value measured at 283.3nm and the lead content is proportional to a certain concentration range, compared with standard series quantified.
10 Reagents and materials
Unless otherwise indicated, the reagents of the present method are excellent pure water to two water with GB/T 6682 provisions.
10.1 Reagents
10.1.1 nitric acid (HNO3).
10.1.2 ammonium dihydrogen phosphate (NH4H2PO4).
10.1.3 the preparation of food simulants reagents required. According to GB 31604.1 requirements.
10.2 reagent preparation
10.2.1 food simulants. formulated in accordance with the provisions of GB 5009.156.
10.2.2 nitric acid solution (95 + 5). Measure 50mL of nitric acid, was added to 950mL water, and mix.
10.2.3 nitric acid solution (1 + 9). Measure 50mL of nitric acid, was added to 450mL water, and mix.
10.2.4 ammonium dihydrogen phosphate solution (20g/L). Weigh 2.0g of ammonium dihydrogen phosphate, dissolved in water, the volume to 100mL.
10.3 Standards
Lead nitrate [Pb (NO3) 2, CAS No. 10099-74-8]. purity> 99.99%, or certified by the National Standards and granted a certificate
Given concentration of lead standard solution.
10.4 Standard Preparation
10.4.1 lead standard stock solution (1000mg/L). Accurately weigh 1.5985g (accurate to 0.0001g) lead nitrate, a nitric acid solution with a small amount
(9 + 1) dissolved into 1000mL volumetric flask, add water to volume, and mix.
10.4.2 intermediate lead standard solution (1.00mg/L). a solution of lead draw stock standard solution 1.00mL to 1000mL volumetric flask, add nitric acid
(95 + 5) to volume, and mix.
10.4.3 lead standard solution series. Pipette intermediate lead standard solution (1.00mg/L) 0mL, 0.500mL, 1.00mL, 2.00mL,
4.00mL, 6.00mL in 100mL volumetric flask, add the appropriate food simulant to volume, and mix. This concentration of lead standard solution series of points
Do is 0μg/L, 5.00μg/L, 10.0μg/L, 20.0μg/L, 40.0μg/L, 60.0μg/L. Note. The sensitivity of the instrument, and the actual concentration of lead in the linear range of the soaking solution to determine the specific concentration of the standard series of lead. If the selected food mold
Quasi was neutral or basic, the need to add an appropriate amount of nitric acid solution of nitric acid in a concentration of about 5% (volume fraction).
11 instruments and equipment
Note. All glassware required nitric acid solution (1 + 5) soaked overnight, washed repeatedly with water and finally water rinse.
11.1 graphite furnace atomic absorption spectrometer. with graphite furnace atomizer, lead hollow cathode lamp.
11.2 Analytical Balance. a sense of the amount of 0.1mg.
12 analysis steps
12.1 Pretreatment of sample
Depending on the intended use conditions and sample to be tested, in accordance with a predetermined GB 5009.156 31604.1 and GB migration test methods and test
Experimental conditions for migration testing. After soaking solution was thoroughly mixed, take part soak test solution for analysis. When the soaking test solution is neutral or alkaline, then
Add appropriate amount of nitric acid in the test solution concentration of nitric acid is about 5% (volume fraction). While doing the blank test specimen.
12.2 Determination
12.2.1 instrument reference conditions
Instrument Reference conditions shown in Table A. 1.
12.2.2 standard curve prepared
The lead concentration according to standard series solution and 10μL 5μL ammonium dihydrogen phosphate solution (20g/L) (the optimum injection volume can be determined according to the instrument used) in the order from low to high while injecting graphite furnace, the absorbance was measured , a concentration series of the standard as abscissa, corresponding to the absorbance
A standard curve for the vertical axis.
12.2.3 Determination of sample solution
The 10μL sample or blank solution and the leaching solution 5μL ammonium dihydrogen phosphate solution (20g/L) (the optimum injection volume can be determined according to the instrument used) simultaneously injected graphite furnace, the absorbance value measured for atomization, and standard quantitative comparison of series.
13 expression analysis results
Obtained from the standard curve the concentration of lead in a sample solution according to GB 5009.156 migration calculating the blank value, then the food to give
Touch migration of lead material and product. The results rounded to three significant figures.
14. Precision
The absolute difference between two measurement results obtained under repeatable conditions not exceed 20% of the arithmetic mean.
Other 15
The detection limit was 0.6μg/L, limit of quantification was 2.0μg/L.
The second Inductively Coupled Plasma Mass Spectrometry
See GB 31604.49.
The third method of inductively coupled plasma emission spectrometry
See GB 31604.49.
The fourth Flame Atomic Absorption Spectrometry
Principle 16
Using food simulants and soaking food contact materials in contact with food products contemplated portion soaking solution by flame atomization, in
Absorbance measured at 283.3nm and the lead content is proportional to a certain concentration range, compared with standard series quantified.
17 Reagents and materials
Unless otherwise indicated, the reagents of the present method are excellent pure water to two water with GB/T 6682 provisions.
17.1 Reagents
17.1.1 nitric acid (HNO3).
17.1.2 the preparation of food simulants reagents required. in accordance with the provisions of GB 31604.1.
17.2 reagent preparation
17.2.1 food simulants. formulated in accordance with the provisions of GB 5009.156.
17.2.2 nitric acid solution (95 + 5). Measure 50mL of nitric acid, was added to 950mL water, and mix.
17.2.3 nitric acid solution (1 + 9). Measure 50mL of nitric acid, was added to 450mL water, and mix.
17.3 Standards
Lead nitrate [Pb (NO3) 2, CAS No. 10099-74-8]. purity> 99.99%, or certified by the National Standards and granted a certificate
Given concentration of lead standard solution.
17.4 Standard Preparation
17.4.1 lead standard stock solution (1000mg/L). Accurately weigh 1.5985g (accurate to 0.0001g) lead nitrate, a nitric acid solution with a small amount
(9 + 1) dissolved into 1000mL volumetric flask, add water to volume, and mix.
17.4.2 intermediate lead standard solution (10.0mg/L). lessons 1.00mL in 100mL volumetric flask, add a solution of lead nitrate standard stock solution (5+
95) to volume, and mix.
17.4.3 lead standard solution series. Pipette intermediate lead standard solution (10.0mg/L) 0mL, 0.500mL, 1.00mL, 2.00mL,
3.00mL, 4.00mL in 10.0mL volumetric flask, add the appropriate food simulant to volume, and mix. This concentration of lead standard solution series of points
Do is 0mg/L, 0.500mg/L, 1.00mg/L, 2.00mg/L, 3.00mg/L, 4.00mg/L.
Note. The sensitivity of the instrument, and the actual concentration of lead in the linear range of the soaking solution to determine the specific concentration of the standard series of lead. If the selected food mold
Quasi was neutral or basic, the need to add an appropriate amount of nitric acid solution of nitric acid in a concentration of about 5% (volume fraction).
18 instruments and equipment
Note. All glassware required nitric acid solution (1 + 5) soaked overnight, washed repeatedly with water and finally water rinse.
18.1 Flame Atomic Absorption Spectrometer. with flame atomizer, lead hollow cathode lamp.
18.2 Analytical Balance. a sense of the amount of 0.1mg.
19 analysis steps
19.1 Pretreatment of sample
With 5.1.
19.2 Determination
19.2.1 instrument reference conditions
Instrument Reference conditions shown in Table B. 1.
19.2.2 standard curve prepared
From low to high a concentration of the order of the series of lead standard solution was measured by flame atomic absorption spectrometer, the absorbance obtained. A standard system
Column solution concentration as the abscissa corresponding to the ordinate is the absorbance standard curve.
19.2.3 Determination of sample solution
The blank solution and the sample were introduced into a soaking liquor flame atomic absorption spectrometer, quantitative comparison with standard curves.
20 expression analysis results
Obtained from the standard curve the concentration of lead in a sample solution, calculated in accordance with migration GB 5009.156 the blank value, to obtain food
Migration of the contact material and the lead article. The results rounded to three significant figures.
21 precision
The absolute difference between two measurement results obtained under repeatable conditions not exceed 10% of the arithmetic mean.
Other 22
The detection limit is...