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GB 5009.11-2014 English PDF (GB5009.11-2014)

GB 5009.11-2014 English PDF (GB5009.11-2014)

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GB 5009.11-2014: National Food Safety Standard -- Determination of total arsenic and abio-arsenic in food

The first section of this Standard specifies the method for the determination of total arsenic in food. The second section of this Standard specifies determination of abio-arsenic content in food by liquid chromatography - atomic fluorescence spectrometry, liquid chromatography - inductively coupled plasma mass spectrometry.
GB 5009.11-2014
GB
NATIONAL STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
National Food Safety Standard
Determination of total arsenic and abio-arsenic in food
ISSUED ON. SEPTEMBER 21, 2015
IMPLEMENTED ON. MARCH 21, 2016
Issued by. National Health and Family Planning Commission of the
PEOPLE Republic of China
Table of Contents
Foreword ... 4
1 Scope ... 5
Section 1. Determination of total arsenic ... 5
Method 1. Inductively coupled plasma mass spectrometry ... 5
2 Principle... 5
3 Reagents and materials ... 6
4 Instruments and apparatuses ... 7
5 Analysis step ... 7
6 Analysis results presentation ... 9
7 Precision... 10
8 Other ... 10
Method 2. Hydride generation atomic fluorescence spectrometry ... 10
9 Principle... 10
10 Reagents and materials... 10
11 Instruments and apparatuses ... 12
12 Analysis steps ... 12
13 Analysis results presentation ... 14
14 Precision ... 14
15 Detection limit ... 15
Method 3. Silver salt method... 15
16 Principle... 15
17 Reagents and materials... 15
18 Instruments and apparatuses ... 17
19 Sample preparation ... 18
20 Analysis steps ... 21
21 Analysis results presentation ... 22
22 Precision ... 22
23 Detection limit ... 22
Section 2. Determination of abio-arsenic in food... 23
Method 1. Liquid chromatography - atomic fluorescence spectrometry (LC-AFS) ... 23
24 Principle... 23
25 Reagents and materials... 23
26 Instruments and apparatuses ... 25
27 Analysis steps ... 25
28 Analysis results presentation ... 28
29 Precision ... 28
30 Other ... 28
31 Principle... 29
32 Reagents and materials... 29
33 Instruments and apparatuses ... 30
34 Analysis steps ... 31
35 Analysis results presentation ... 32
36 Precision ... 33
37 Other ... 33
Appendix A Microwave Digestion reference conditions ... 34
Appendix B Chromatogram ... 36
Foreword
This Standard replaces GB/T 5009.11-2003 "National food safety standard - Determination of total arsenic and abio-arsenic in food."
Compared with GB/T 5009.11-2003, the main changes of this Standard are as follows.
- CHANGE the standard name to ?€?National food safety standard -
Determination of total arsenic and abio-arsenic in food?€?.
- DELETE the arsenic stain method and borohydride reduction colorimetric method for the determination of total arsenic in food; DELETE the atomic fluorescence method and the silver salt method for the determination of abio-arsenic in food.
- ADD the inductively coupled plasma mass spectrometry (ICP-MS) for the determination of total arsenic in food;
- ADD the liquid chromatography - atomic fluorescence spectrometry (LC- AFS) and liquid chromatography - inductively coupled plasma mass
spectrometry (LC-ICP-MS) for the determination of abio-arsenic in food. National food safety standard
Determination of total arsenic and abio-arsenic in food
1 Scope
The first section of this Standard specifies the method for the determination of total arsenic in food. The second section of this Standard specifies
determination of abio-arsenic content in food by liquid chromatography - atomic fluorescence spectrometry, liquid chromatography - inductively coupled plasma mass spectrometry.
The method 1, method 2 AND method 3 of this Standard?€?s first section apply to the determination of total arsenic in various foods. The second section applies to the determination of abio-arsenic (including arsenate and arsenite) content in rice, aquatic animals, infant cereals complementary food, canned infant complementary food.
Section 1. Determination of total arsenic
Method 1. Inductively coupled plasma mass
spectrometry
2 Principle
The sample is treated through acid digestion to produce sample solution, which is atomized and sent by a carrier gas into ICP torch; after evaporation, dissociation, atomization and ionization process, etc., it is converted into electrically charged ions, which is sent into the mass spectrometer by ion- collection system; AND it is separated by the mass spectrometer based on their mass-to-charge ratio. As for certain mass-to-charge ratio, the mass spectrum?€?s signal intensity is proportional to the number of ions entering into the mass spectrometer, i.e., the sample concentration is proportional to the mass spectrum?€?s signal intensity. By measuring the mess spectrum?€?s signal intensity, the arsenic in the sample solution is measured.
3 Reagents and materials
Note. Unless otherwise specified, the reagent used in this method is analytically pure; AND the water is grade I water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3). MOS level (dedicated high-purity chemicals for electronics industry), BV (III) level.
3.1.2 Hydrogen peroxide (H2O2).
3.1.3 MS tuning solution. Li, Y, Ce, Ti, Co, recommended concentration is 10ng/mL.
3.1.4 Internal standard stock solution. Ge, concentration is 100??g/mL.
3.1.5 Sodium hydroxide (NaOH).
3.2 Reagent preparation
3.2.1 Nitric acid solution (2 + 98). MEASURE 20mL of nitric acid; POUR it slowly into 980mL of water; MIX it uniformly.
3.2.2 Internal standard solution Ge or Y (1.0??g/mL). TAKE 1.0mL of internal standard solution; USE nitric acid solution (2 + 98) to dilute it AND make the volume reach to 100mL.
3.2.3 Sodium hydroxide solution (100g/L). WEIGH 10.0g of sodium hydroxide; USE water to dissolve it AND make the volume reach to 100mL.
3.3 Standard substance
Standard arsenic trioxide (As2O3). purity ??? 99.5%.
3.4 Standard Solution preparation
3.4.1 Arsenic standard stock solution (100mg/L, based on As). accurately WEIGH 0.0132g of arsenic trioxide which has been dried at 100??C for 2h; ADD 1mL of sodium hydroxide solution (100g/L) and a small amount of water to dissolve it; TRANSFER it into a 100mL volumetric flask; ADD appropriate amount of hydrochloric acid to adjust its pH to near neutral; USE water to dilute it to the mark. PRESERVE it at 4??C in dark, AND the preservation period is 1 year. Or otherwise PURCHASE a standard solution material which is certified nationally AND awarded with standard substance certificate.
3.4.2 Arsenic standard solution (1.00mg/L, based on As). accurately PIPETTE 0.5g (accurate to 0.001g) of sample into digestion tank, ADD 5mL of nitric acid, SETTLE for 30min; COVER safety valve; ...

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