GB 5009.12-2023 PDF English
US$230.00 · In stock · Download in 9 secondsGB 5009.12-2023: National food safety standard - Determination of lead in foods Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB 5009.12: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.12-2023 | English | 230 |
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National food safety standard - Determination of lead in foods
| Valid |
| GB 5009.12-2017 | English | 85 |
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National food safety standard -- Determination of lead in food
| Obsolete |
| GB 5009.12-2010 | English | 140 |
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National food safety standard -- Determination of lead in foods
| Obsolete |
| GB/T 5009.12-2003 | English | 559 |
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4 days
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Determination of lead in foods
| Obsolete |
| GB/T 5009.12-1996 | English | 279 |
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3 days
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Method for determination of lead in foods
| Obsolete |
| GB 5009.12-1985 | English | 199 |
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2 days
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Method for determination of lead in foods
| Obsolete |
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GB 5009.12-2023: National food safety standard - Determination of lead in foods---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB5009.12-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Determination of lead in
foods
Issued on. SEPTEMBER 06, 2023
Implemented on. MARCH 06, 2024
Issued by. National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
2 Principle... 4
3 Reagents and materials... 4
4 Instruments and apparatuses... 6
5 Analysis steps... 6
6 Expression of analysis results... 8
7 Precision... 9
8 Others... 9
9 Principle... 10
10 Reagents and materials... 10
11 Instruments and apparatuses... 11
12 Analysis steps... 12
13 Expression of analysis results... 13
14 Precision... 13
15 Others... 13
Appendix A Microwave digestion heating program... 14
Appendix B Desalted sample operation steps... 15
Appendix C Apparatus reference conditions for graphite furnace atomic absorption
spectrometry... 17
Appendix D Apparatus reference conditions for flame atomic absorption spectrometry
... 18
Foreword
This Standard replaces GB 5009.12-2017 Food safety national standard -
Determination of lead in food.
Compared with GB 5009.12-2017, the major changes of this Standard are as follows.
-- Add the pretreatment method for samples that need to be desalted in Method 1 –
Graphite furnace atomic absorption spectrometry;
-- Remove Method 4 – Dithizone colorimetry;
-- Modify the detection limit and quantitation limit of Method 1 – Graphite furnace
atomic absorption spectrometry.
National food safety standard - Determination of lead in
foods
1 Scope
This Standard specifies the methods for the determination of lead in foods by graphite
furnace atomic absorption spectrometry, inductively coupled plasma mass spectrometry
and flame atomic absorption spectrometry.
This Standard applies to the determination of lead in foods.
Method 1 – Graphite furnace atomic absorption spectrometry
2 Principle
After digestion treatment, the sample is atomized in a graphite furnace and the
absorbance is measured at 283.3 nm. Within a certain concentration range, the
absorbance value of lead is proportional to the lead content and can be compared
quantitatively with the standard series.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are guaranteed reagents, and
the water is grade-II water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Perchloric acid (HClO4).
3.1.3 Ammonium dihydrogen phosphate (NH4H2PO4).
3.1.4 Palladium nitrate [Pd(NO3)2].
3.1.5 Ammonium acetate (CH3COONH4).
3.1.6 Sodium acetate (CH3COONa).
3.2 Preparation of reagents
3.2.1 Nitric acid solution (5+95). Measure 50 mL of nitric acid; slowly add it to 950
mL of water; mix well.
3.2.2 Nitric acid solution (1+9). Measure 50 mL of nitric acid; slowly add it to 450 mL
of water; mix well.
3.2.3 Nitric acid solution (1+99). Measure 10 mL of nitric acid; slowly add it to 990
mL of water; mix well.
3.2.4 Sodium acetate solution (2 mol/L). Weigh 164.0 g of sodium acetate; add water
to dissolve; adjust the volume to 1 000 mL.
3.2.5 Ammonium acetate solution (1 mol/L). Weigh 77.1 g of ammonium acetate; add
water to dissolve; adjust the volume to 1 000 mL.
3.2.6 Ammonium dihydrogen phosphate-palladium nitrate solution. Weigh 0.02 g of
palladium nitrate; add a small amount of nitric acid solution (1+9) to dissolve it; then,
add 2 g of ammonium dihydrogen phosphate; after dissolution, use nitric acid solution
(5+95) to adjust the volume to 100 mL; mix well.
3.3 Standard
Lead nitrate [Pb(NO3)2, CAS number. 10099-74-8]. purity >99.99%, or lead standard
solution certified by the state and granted with a reference material certificate.
3.4 Preparation of standard solution
4 Instruments and apparatuses
Note. All glassware and polytetrafluoroethylene digestion inner tanks need to be soaked
in nitric acid solution (1+5) or nitric acid solution (1+4) overnight, rinsed
repeatedly with tap water, and finally rinsed with water and dried.
4.1 Atomic absorption spectrometer. equipped with graphite furnace atomizer and
accompanied by lead hollow cathode lamp.
4.2 Analytical balance. The sensitivity is 0.1 mg and 1 mg, respectively.
4.5 Constant-temperature drying oven.
4.6 Pressure digestion tank. equipped with polytetrafluoroethylene digestion inner tank.
4.7 Solid-phase extraction column.
5 Analysis steps
5.1 Sample preparation
5.1.1 Solid samples
5.1.2 Liquid samples
For samples of soft drinks, alcoholic beverages, condiments, etc., shake well.
5.1.3 Semi-solid samples
Mix well.
5.2 Sample pretreatment
5.3 Determination
5.3.1 Apparatus reference conditions
See Appendix C for apparatus reference conditions.
5.3.2 Preparation of standard curve
In order of mass concentration from low to high, add 10 μL of lead standard series
solution and 5 μL of ammonium dihydrogen phosphate-palladium nitrate solution (the
optimal injection volume and optimal matrix modifier can be determined according to
the instrument used, and samples passing through the solid-phase extraction column do
not need to be added with matrix modifier) into the graphite furnace at the same time,
and measure their absorbance values after atomization.
6 Expression of analysis results
The content of lead in the sample is calculated according to Formula (1).
7 Precision
When the lead content in the sample is greater than 1 mg/kg, the absolute difference
between the two independent measurement results obtained under repeatability
conditions shall not exceed 10% of the arithmetic mean; when it is less than or equal to
1 mg/kg and greater than 0.1 mg/kg,
8 Others
When the sample volume is 0.5 g (or 0.5 mL) and the constant volume is 10 mL, the
detection limit of the method is 0.02 mg/kg (or 0.02 mg/L), and the quantitation limit
is 0.04 mg/kg (or 0.04 mg/ L).
For samples such as raw milk, pasteurized milk, sterilized milk, fruit and vegetable
juices and their beverages [excluding fruit and vegetable juices containing berries and
small fruits, as well as their beverages, and concentrated fruit and vegetable juices
(pulp)], liquid infant and young child formula foods, etc., when the sample volume is 2
g (or 2 mL) and the constant volume is 10 mL, the detection limit of the method is 0.005
mg/kg (or 0.005 mg/L), and the quantitation limit is 0.01 mg/kg (or 0.01 mg/L).
9 Principle
After the sample is processed, lead ions form a complex with sodium
diethyldithiocarbamate (DDTC) under certain pH conditions, which is extracted and
separated by 4-methyl-2-pentanone (MIBK) and introduced into the atomic absorption
spectrometer. After flame atomization, measure the absorbance at 283.3 nm. Within a
certain concentration range, the absorbance value of lead is proportional to the lead
content and can be compared quantitatively with the standard series.
10 Reagents and materials
Unless otherwise specified, all the reagents used in this method are analytical reagents,
and the water used is grade-II water as specified by GB/T 6682.
10.1 Reagents
10.1.1 Nitric acid (HNO3). guaranteed reagent.
10.1.2 Perchloric acid (HClO4). guaranteed reagent.
10.1.3 Ammonium sulfate [(NH4)2SO4].
10.1.4 Ammonium citrate [C6H5O7(NH4)3].
10.1.5 Bromothymol blue (C27H28O5SBr2).
10.1.6 Sodium diethyldithiocarbamate [DDTC, (C2H5)2NCSSNa·3H2O].
10.1.7 Ammonia (NH3·H2O). guaranteed reagent.
10.1.8 4-Methyl-2-pentanone (MIBK, C6H12O).
10.1.9 Hydrochloric acid (HCl). guaranteed reagent.
10.2 Preparation of reagents
10.3 Standard
Lead nitrate [Pb(NO3)2, CAS number. 10099-74-8]. purity >99.99%, or lead standard
solution certified by the state and granted with a reference material certificate.
10.4 Preparation of standard solution
10.4.1 Lead standard stock solution (1 000 mg/L). Accurately weigh 1.598 5 g (accurate
to 0.000 1 g) of lead nitrate; use a small amount of nitric acid solution (1+9) to dissolve
it; transfer it to a 1 000 mL volumetric flask; add water to the mark; mix well.
10.4.2 Lead standard working solution (10.0 mg/L). Accurately draw 1.00 mL of lead
standard stock solution (1 000 mg/L) into a 100 mL volumetric flask; add nitric acid
solution (5+95) to the mark; mix well.
11 Instruments and apparatuses
Note. All glassware needs to be soaked in nitric acid solution (1+5) or nitric acid
solution (1+4) overnight, rinsed repeatedly with tap water, and finally rinsed
with water and dried.
11.1 Atomic absorption spectrometer. equipped with flame atomizer and accompanied
by lead hollow cathode lamp.
11.2 Analytical balance. The sensitivity is 0.1 mg and 1 mg, respectively.
11.3 Adjustable electric furnace and adjustable electric hot plate.
12 Analysis steps
12.1 Sample preparation
Same as 5.1.
12.2 Sample pretreatment
Same as 5.2.1.
12.3 Determination
12.3.1 Apparatus reference conditions
See Appendix D for apparatus reference conditions.
12.3.2 Preparation of standard curve
Respectively draw 0 mL, 0.25 mL, 0.50 mL, 1.00 mL, 1.50 mL and 2.00 mL of lead
standard working solution (equivalent to 0 μg, 2.50 μg, 5.00 μg, 10.0 μg, 15.0 μg and
20.0 μg of lead) into 125 mL separatory funnels; add additional water to 60 mL. Add 2
mL of ammonium citrate solution (250 g/L), 3 ~ 5 drops of bromothymol blue aqueous
solution (1 g/L); use ammonia solution (1+1) to adjust the pH until the solution changes
from yellow to blue; add 10 mL of ammonium sulfate solution (300 g/L) and 10 mL of
DDTC solution (50 g/L); shake well. Leave it for about 5 minutes; add 10 mL of MIBK;
shake vigorously for extraction for 1 min; let it stand for layering; discard the water
layer; put the MIBK layer into a 10 mL graduated tube with a stopper to obtain a
standard series of solutions.
13 Expression of analysis results
The content of lead in the sample is calculated according to Formula (2).
14 Precision
The absolute difference of two independent test results obtained under repeatability
cannot exceed 10% of the arithmetic mean value.
15 Others
When the sample volume is 0.5 g (or 0.5 mL), the detection limit of the method is 0.4
mg/kg (or 0.4 mg/L), and the quantification limit is 1.2 mg/kg (or 1.2 mg/L).
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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