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GB 5009.11-2024 English PDF (GB5009.11-2024)

GB 5009.11-2024 English PDF (GB5009.11-2024)

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GB 5009.11-2024: National food safety standards--Determination of total arsenic and inorganic arsenic in food
GB 5009.11-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
GB 5009.11-2024
National food safety standard - Determination of total
arsenic and inorganic arsenic in food
ISSUED ON: FEBRUARY 08, 2024
IMPLEMENTED ON: AUGUST 08, 2024
Issued by: National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword ... 4
1 Scope ... 5
Chapter 1: Determination of total arsenic in food ... 5
Method I: Hydride generation atomic fluorescence spectrometry ... 5
2 Principle ... 5
3 Reagents and materials ... 6
4 Instruments and equipment ... 8
5 Analysis procedure ... 8
6 Expression of analysis results ... 11
7 Precision ... 11
8 Others ... 12
Method II: Inductively coupled plasma mass spectrometry ... 12
Method III: Graphite furnace atomic absorption spectrometry ... 12
9 Principle ... 12
10 Reagents and materials ... 12
11 Instruments and equipment ... 13
12 Analysis procedure ... 14
13 Expression of analysis results ... 15
14 Precision ... 15
15 Others ... 16
Chapter 2: Determination of inorganic arsenic in food ... 16
Method I: Liquid chromatography-atomic fluorescence spectrometry ... 16
16 Principle ... 16
17 Reagents and materials ... 16
18 Instruments and equipment ... 19
19 Analysis procedure ... 20
20 Expression of analysis results ... 25
21 Precision ... 25
22 Others ... 26
Method II: Liquid chromatography-inductively coupled plasma mass spectrometry . 26
23 Principle ... 26
24 Reagents and materials ... 26
25 Instruments and equipment ... 29
26 Analysis procedure ... 29
27 Expression of analysis results ... 32
28 Precision ... 33
29 Others ... 33
Annex A Reference conditions for microwave digestion ... 34
Annex B Reference conditions for instruments ... 35
Annex C Reference conditions for instruments ... 36
Annex D Chromatograms of LC-AFS method ... 38
Annex E Chromatograms of LC-ICP/MS method ... 42
National food safety standard - Determination of total
arsenic and inorganic arsenic in food
1 Scope
Chapter 1 of this Standard specifies the methods for the determination of total arsenic
in food.
Methods I and II of Chapter 1 of this Standard apply to the determination of total arsenic
in food. Method III applies to the determination of total arsenic in food (except milk
powder and prepared milk powder, oils and fats and their products, condiments, and
special dietary foods).
Chapter 2 of this Standard specifies the methods for the determination of inorganic
arsenic in food.
Chapter 2 of this Standard applies to the determination of inorganic arsenic in cereals
and their products, aquatic animals and their products, edible fungi and their products,
oils and fats and their products, condiments, supplementary foods for infants and young
children, algae and their products.
Chapter 1: Determination of total arsenic in food
Method I: Hydride generation atomic fluorescence
spectrometry
2 Principle
After the sample is digested, thiourea is added to pre-reduce the pentavalent arsenic to
trivalent arsenic, and then sodium borohydride or potassium borohydride is added to
reduce the trivalent arsenic to generate arsine, which is loaded into the quartz atomizer
by argon gas and decomposed into atomic arsenic. The atomic arsenic produces atomic
fluorescence under the excitation of the emitted light of the arsenic hollow cathode lamp.
Under fixed conditions, its fluorescence intensity is proportional to the arsenic
concentration in the solution being tested. It is quantitatively determined by external
standard method.
3.2.5 Magnesium nitrate solution (150 g/L): Weigh 15.0 g of magnesium nitrate,
dissolve with water and dilute to 100 mL, and mix well.
3.2.6 Hydrochloric acid solution (1 + 1): Measure 100 mL of hydrochloric acid, slowly
pour it into 100 mL of water, and mix well.
3.2.7 Sulfuric acid solution (1 + 9): Measure 100 mL of sulfuric acid, slowly pour it
into 900 mL of water, and mix well.
3.2.8 Nitric acid solution (2 + 98): Measure 20 mL of nitric acid, slowly pour it into
980 mL of water, and mix well.
NOTE: This method can also use sodium borohydride (20 g/L) as the reducing agent: weigh 20 g of
sodium borohydride, dissolve it in 1000 mL of 5 g/L sodium hydroxide solution, and mix well. The
concentration of potassium borohydride or sodium borohydride solution can be adjusted according
to the sensitivity of the instrument. Freshly prepare each time before use.
3.3 Reference material
Arsenic trioxide (As2O3, CAS number: 1327-53-3) reference material: purity ≥ 99.5 %.
3.4 Preparation of standard solutions
3.4.1 Arsenic standard stock solution (100 mg/L, calculated as As): Accurately weigh
0.0132 g of arsenic trioxide that has been dried at 100 °C for 2 h, add 1 mL of sodium
hydroxide solution (100 g/L) and a small amount of water to dissolve, transfer to a 100
mL volumetric flask, add an appropriate amount of hydrochloric acid to adjust its
acidity to near neutral, and dilute to the mark with water. Store in a refrigerator at 2 ℃
~ 8 ℃ away from light, the validity period is 1 year. Or arsenic standard solution
certified by the country and awarded a reference material certificate.
3.4.2 Arsenic standard use solution (1.00 mg/L, calculated as As): Accurately pipette
1.00 mL of arsenic standard stock solution (100 mg/L) into a 100 mL volumetric flask,
and dilute to the mark with nitric acid solution (2 + 98). Store in a refrigerator at 2 ℃
~ 8 ℃ away from light, the validity period is 3 months.
3.4.3 Arsenic standard series solutions: Take 7 25 mL volumetric flasks or colorimetric
tubes, accurately add 0.00 mL, 0.05 mL, 0.10 mL, 0.25 mL, 0.50 mL, 1.50 mL and 3.00
mL of arsenic standard use solution (1.00 mg/L) in sequence (equivalent to arsenic
concentrations of 0.0 μg/L, 2.0 μg/L, 4.0 μg/L, 10.0 μg/L, 20.0 μg/L, 60.0 μg/L and
120.0 μg/L respectively), add 12.5 mL of sulfuric acid solution (1 + 9) and 2 mL of
thiourea + ascorbic acid solution, add water to the mark, mix well, and let stand for 30
min before determination. Freshly prepare each time before use.
NOTE: The mass concentration range of arsenic in the standard series solutions can be fine-tuned
according to the sensitivity of the instrument and the actual arsenic content in the sample.
For thawed quick-frozen food, it shall take the edible parts and crush evenly; for canned
food, it shall crush or homogenize evenly.
5.1.2 Liquid samples
For samples such as beverages, condiments, milk and their products, oils and fats and
their products, it shall homogenize.
5.1.3 Semi-solid samples
Stir evenly.
5.2 Digestion of samples
5.2.1 Wet digestion
Weigh 0.5 g ~ 2.5 g (accurate to 0.001 g) of solid samples or 5.0 g ~ 10.0 g (accurate to
0.001 g) of liquid samples into a digestion bottle or digestion tube, add 20 mL of nitric
acid, 4 mL of perchloric acid and 1.25 mL of sulfuric acid and leave overnight. The next
day, heat and digest at 120 ℃ ~ 200 ℃ step by step. If there are still undecomposed
substances or the color becomes darker when the digestion solution reaches about 5 mL,
add 5 mL ~ 10 mL of nitric acid, and then digest to about 2 mL. Repeat this 2 to 3 times,
taking care to avoid carbonization, and continue heating and digestion until the
digestion solution is about 1 mL, which is colorless and clear, and the digestion bottle
or digestion tube is filled with white smoke (fo...
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