GB 5009.11-2024 PDF English
US$470.00 · In stock · Download in 9 secondsGB 5009.11-2024: National food safety standard - Determination of total arsenic and inorganic arsenic in food Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB 5009.11: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.11-2024 | English | 470 |
Add to Cart
|
0-9 seconds. Auto-delivery
|
National food safety standard - Determination of total arsenic and inorganic arsenic in food
| Valid |
| GB 5009.11-2014 | English | 145 |
Add to Cart
|
0-9 seconds. Auto-delivery
|
National food safety standard - Determination of total arsenic and abio-arsenic in food
| Obsolete |
| GB/T 5009.11-2003 | English | 150 |
Add to Cart
|
0-9 seconds. Auto-delivery
|
Determination of total arsenic and abio-arsenic in foods
| Obsolete |
| GB/T 5009.11-1996 | English | 319 |
Add to Cart
|
3 days
|
Method for determination of total arsenic in food
| Obsolete |
| GB 5009.11-1985 | English | 239 |
Add to Cart
|
2 days
|
Method for determination of total arsenic in foods
| Obsolete |
Excerpted PDFs (Download full copy in 9 seconds upon purchase)PDF Preview: GB 5009.11-2024
GB 5009.11-2024: National food safety standard - Determination of total arsenic and inorganic arsenic in food
---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/GB5009.11-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
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
Part 1.Determination of total arsenic in food... 5
Method 1 -- 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 2 -- Inductively coupled plasma mass spectrometry... 12
Method 3 -- Graphite furnace atomic absorption spectrometry... 12
9 Principle... 12
1 Scope
Part 1 of this Standard specifies the methods for the determination of total arsenic in
food.
Methods I and II of Part 1 of this Standard apply to the determination of total arsenic in
food. Method 3 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).
Part 2 of this Standard specifies the methods for the determination of inorganic arsenic
in food.
Part 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.
Part 1.Determination of total arsenic in food
Method 1 -- 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 Reagents and materials
Unless otherwise stated, the reagents used in this method are analytical reagents, and
the water is Grade 1 water specified in GB/T 6682.
3 Reagents
4 Instruments and equipment
4.1 Atomic fluorescence spectrometer.
4.2 Electronic balance. the minimum division is 0.01 mg, 0.1 mg and 1 mg.
4.3 Homogenizer.
4.4 High-speed crusher.
4.5 Electrothermal digestion device. temperature-controlled electric heating plate or
graphite digestion instrument, the maximum temperature is not less than 350 ℃, and
the temperature control accuracy is ±5 ℃.
4.6 Muffle furnace.
4.7 Constant temperature drying oven. the temperature control accuracy is ±2 ℃.
4.8 Microwave digestion system. it is equipped with polytetrafluoroethylene digestion
inner tank.
4.9 Pressure digestion tank.
NOTE. Glassware and polytetrafluoroethylene digestion inner tanks need to be soaked in (1 + 4)
nitric acid solution for 24 h, rinsed repeatedly with tap water, and finally rinsed with water.
5 Analysis procedure
5.1 Preparation of samples
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 (for samples of aquatic animals and their
products, edible fungi and their products, fish oil and their products, krill oil and their
products, algae and their products which have high organic arsenic, raise the digestion
temperature to 280 ℃ ~ 300 ℃ and continue to heat and digest until the digestion
solution is about 0.5 mL, which is colorless and clear, and the digestion bottle or
digestion tube is filled with white smoke). After cooling, slowly add about 10 mL of
water along the wall of the digestion container, and then evaporate until the digestion
bottle or digestion tube is filled with white smoke. Cool down, transfer the digestion
solution with water into a 25 mL volumetric flask or colorimetric tube, add 2 mL of
thiourea + ascorbic acid solution, dilute to the mark with water, mix well, and leave it
for 30 min before determination. Do a blank test at the same time.
5.2.2 Dry ashing method
Weigh 1.0 g ~ 2.5 g (accurate to 0.001 g) of solid samples or weigh 4.0 g (accurate to
0.001 g) of liquid samples (excluding samples of oils and fats), and place it in a 50 mL
~ 100 mL crucible. Add 10 mL of magnesium nitrate solution (150 g/L) and mix well,
evaporate to dryness over low heat, and cover the dry residue with 1 g of magnesium
oxide (for samples of oils and fats, weigh 1.00 g in a 50 mL ~ 100 mL crucible, and
directly add 0.2 g of magnesium oxide to cover on oils and fats), carbonize on an electric
furnace until there is no black smoke, then transfer it to a 550 ℃ muffle furnace for
ashing for 4 h. Take it out and let it cool, carefully add 5 mL ~ 10 mL of hydrochloric
acid solution (1 + 1) to neutralize the magnesium oxide and dissolve the ash, transfer it
to a 25 mL volumetric flask or colorimetric tube, add 2 mL of thiourea + ascorbic acid
solution to the volumetric flask or colorimetric tube, wash the crucible with sulfuric
acid solution (1 + 9) in batches, combine the washing liquids and dilute to the mark,
mix well, and leave it for 30 min before determination. Do a blank test at the same time.
5.2.3 Microwave digestion method
Weigh 0.2 g ~ 0.8 g (accurate to 0.001 g) of solid samples and samples of oils and fats
and their products, or weigh 1.0 g ~ 3.0 g (accurate to 0.001 g) of samples containing
more water or liquid samples into a digestion tank, add 5 mL ~ 8 mL of nitric acid, and
leave it for more than 30 min. For samples that are difficult to digest such as meat, oils,
and fats, add 0.5 mL ~ 1 mL of hydrogen peroxide, cover the safety valve, and put the
digestion tank into the microwave digestion system. According to different types of
samples, set up appropriate microwave digestion procedures (see Annex A, Table A.1),
and perform digestion according to relevant steps. After digestion, reduce acid to 1 mL
~ 2 mL at 135 °C ~ 145 °C. Transfer the digestion solution to a 25 mL volumetric flask
or colorimetric tube, wash the digestion tank 3 times with a small amount of sulfuric
acid solution (1 + 9), combine the washing liquid into the volumetric flask or
colorimetric tube and add 2 mL of thiourea + ascorbic acid solution, dilute to mark with
sulfuric acid solution (1 + 9), mix well, and leave it for 30 min before determination.
Do a blank test at the same time.
5.2.4 Pressure tank digestion method
Weigh 0.2 g ~ 1.0 g (accurate to 0.001 g) of solid samples and samples of oils and fats
and their products, or weigh 1.0 g ~ 5.0 g (accurate to 0.001 g) of fresh samples or
liquid samples into a digestion inner tank, and add 5 mL of nitric acid and soak
overnight. Cover the inner cover, tighten the stainless steel jacket, put it into a constant
temperature drying oven, keep it at 140 ℃ ~ 160 ℃ for 3 h ~ 4 h, naturally cool to
room temperature, then slowly loosen the stainless steel jacket, take out the digestion
inner tank, and place it on a temperature-controlled electric heating plate at 135 ℃ ~
145 ℃ to reduce acid to 1 mL ~ 2 mL. Transfer the digestion solution to a 25 mL
volumetric flask or colorimetric tube, wash the digestion tank 3 times with a small
amount of sulfuric acid solution (1 + 9), combine the washing liquid into the volumetric
flask or colorimetric tube and add 2 mL of thiourea + ascorbic acid solution, dilute to
mark with sulfuric acid solution (1 + 9), mix well, and leave it for 30 min before
determination. Do a blank test at the same time.
NOTE. The pressure tank digestion method does not apply to samples with complex matrices such
as aquatic animals and their products, edible fungi and their products, fish oil, krill oil and their
products, aquatic condiments, algae and their products, which have a high organic arsenic content.
5.3 Reference conditions for instruments
Negative high voltage. 260 V; arsenic hollow cathode lamp current. 50 mA ~ 80 mA;
carrier gas. argon; carrier gas flow rate. 500 mL/min; shielding gas flow rate. 800
mL/min; determination method. fluorescence intensity; reading method. peak area.
5.4 Plotting of standard curve
After the instrument is preheated and stabilized, the reagent blank and standard series
solutions are introduced into the instrument in sequence to determine the atomic
fluorescence intensity. Taking the atomic fluorescence intensity as the ordinate and the
arsenic mass concentration as the abscissa, plot a standard curve and obtain the
regression equation.
5.5 Determination of sample solution
Under the same conditions, introduce the blank solution and sample solution into the
instrument for determination. The mass concentration of arsenic in the sample is
calculated according to the regression equation.
6 Expression of analysis results
The arsenic content in the sample is calculated according to formula (1).
X - the arsenic content in the sample, in milligrams per kilogram (mg/kg);
ρ - the arsenic content in the sample solution, in micrograms per liter (μg/L);
ρ0 - the arsenic content in the blank solution, in micrograms per liter (μg/L);
V - the constant volume of the sample digestion solution, in milliliters (mL);
1000 - the conversion factor;
m - the weighing mass of the sample, in grams (g).
When the arsenic content is ≥ 1.00 mg/kg, the calculation results shall retain 3
significant figures; when the arsenic content is < 1.00 mg/kg, the calculation results
shall retain 2 significant figures.
7 Precision
When the arsenic content in the sample is greater than 1.00 mg/kg, the absolute
difference between the two independent determination results obtained under
repeatability conditions shall not exceed 10 % of the arithmetic mean; when it is less
than or equal to 1.00 mg/kg and greater than 0.10 mg/kg, the absolute difference
between two independent determination results obtained under repeatability conditions
shall not exceed 15 % of the arithmetic mean; when it is less than or equal to 0.10 mg/kg,
the absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 20 % of the arithmetic mean.
8 Others
When the weighing mass of a solid sample is 1.0 g and the constant volume is 25 mL,
the method detection limit is 0.01 mg/kg and the method quantitation limit is 0.04
mg/kg. When the sampling volume of a liquid sample is 2 g and the constant volume is
25 mL, the method detection limit is 0.005 mg/kg and the method quantitation limit is
0.02 mg/kg.
9 Principle
After digestion treatment, the sample is atomized in a graphite furnace and the
absorbance is measured at 193.7 nm. Within a certain concentration range, the
absorbance value of arsenic is proportional to the arsenic content. It is quantitatively
determined by external standard method.
10 Reagents and materials
Unless otherwise stated, the reagents used in this method are guarantee reagents, and
the water is Grade 1 water specified in GB/T 6682.
10.1 Reagents
10.3 Reference material
Arsenic trioxide (As2O3, CAS number. 1327-53-3) reference material. purity ≥ 99.5 %.
10.4 Preparation of standard solutions
11 Instruments and equipment
12 Analysis procedure
12.1 Preparation of samples
Same as 5.1.
12.2 Digestion of samples
12.2.1 Microwave digestion method
Weigh 0.2 g ~ 0.8 g (accurate to 0.001 g) of solid samples and samples of oils and fats
and their products, or weigh 1.0 g ~ 3.0 g (accurate to 0.001 g) of samples containing
more water or liquid samples into a digestion tank; add 5 mL ~ 8 mL of nitric acid and
leave it for more than 30 min. For samples that are difficult to digest such as meat and
aquatic animals and their products, add 0.5 mL ~ 1 mL of hydrogen peroxide, cover the
safety valve, and put the digestion tank into the microwave digestion system. According
to different types of samples, set up appropriate microwave digestion procedures (see
Table A.2) and perform digestion according to relevant steps. After digestion is
completed, reduce acid to 0.5 mL ~ 1 mL at 140 ℃ ~ 145 ℃, dilute with water to 25
mL, and mix well for later use. Do a blank test at the same time.
12.4 Plotting of standard curve
Pipette 20 μL of arsenic standard series solution and 5 μL of palladium nitrate solution
(1 g/L) (the optimal sample injection volume can be determined according to the
instrument used), inject them into a graphite furnace in order of mass concentration
from low to high, and determine the absorbance value after atomization. Taking the
mass concentration as the abscissa and the absorbance as the ordinate to plot a standard
curve.
12.5 Determination of sample solution
Under the same test conditions as the determination of standard solution, pipette 20 μL
of blank solution or sample solution and 5 μL of palladium nitrate solution (the optimal
sample injection volume can be determined according to the instrument used) and inject
them into a graphite furnace, determine the absorbance value after atomization, and
quantitatively determine by comparison with standard series.
13 Expression of analysis results
The arsenic content in the sample is calculated according to formula (2).
14 Precision
Same as Clause 7.
15 Others
When the weighing mass of a solid sample is 0.5 g and the constant volume is 25 mL,
the method detection limit is 0.03 mg/kg and the method quantification limit is 0.09
mg/kg. When the sampling mass of a liquid sample is 2 g and the constant volume is
25 mL, the method detection limit is 0.008 mg/kg and the method quantitation limit is
0.03 mg/kg.
16 Principle
After the inorganic arsenic in the sample is extracted with dilute nitric acid, it is
separated by liquid chromatography. The separated target compound reacts with
potassium borohydride or sodium borohydride in an acidic environment to generate
gaseous arsenic compounds, which are determined with an atomic fluorescence
spectrometer. It is qualitatively determined by retention time and mass-to-charge ratio,
and quantitatively determined by external standard method.
17 Reagents and materials
Unless otherwise stated, the reagents used in this method are guarantee reagents, and
the water is Grade 1 water specified in GB/T6682.
17.1 Reagents
17.2 Preparation of reagents
17.3 Reference materials
17.4 Preparation of standard solutions
18 Instruments and equipment
18.1 Liquid chromatography-atomic fluorescence spectrometer (LC-AFS). it consists
of a liquid chromatograph and an atomic fluorescence spectrometer.
18.2 Tissue homogenizer.
18.3 High-speed crusher.
18.4 Microwave digestion system. it is equipped with microwave extraction tank.
18.5 Centrifuge. speed ≥ 8000 r/min.
18.6 pH meter. the accuracy is 0.01.
18.7 Electronic balance. the minimum division is 0.01 mg, 0.1 mg and 1 mg.
18.8 Constant temperature drying oven. the temperature control accuracy is ±2 °C.
18.9 Ultrasonic cleaner.
18.10 Filter membrane. 0.45 μm.
18.11 Sieve. particle size ≤ 425 μm (sieve opening ≥ 40 mesh).
NOTE. Glassware and microwave extraction inner tanks need to be soaked in (1 + 4) nitric acid
solution for 24 h, rinsed repeatedly with tap water, and finally rinsed with water.
19 Analysis procedure
19.1 Preparation of samples
19.1.1 Solid samples
19.1.2 Liquid samples
For condiments, fats and oils and their products, etc., it shall homogenize.
19.1.3 Semi-solid samples
Stir evenly.
19.2 Extraction of samples
19.2.1 Cereals and their products
19.2.3 Supplementary foods for infants and young children
19.2.6 Oils and fats and their products
Weigh about 0.3 g ~ 1.0 g of the sample (accurate to 0.001 g) into a 50 mL
polypropylene centrifuge tube, and add 20 mL of 0.15 mol/L nitric acid + 0.45 %
hydrogen peroxide solution. Make hot extraction in a thermostat at 90 ℃ for 2.5 h, and
shake for 1 min every 0.5 h. After extraction, take it out and cool it to room temperature,
centrifuge at 8000 r/min for 15 min. The subsequent steps are the same as 19.2.2 “Take
5 mL of the supernatant and place it in a centrifuge tube... do a blank test at the same
time.”
19.2.7 Algae and their products
Weigh about 0.2 g ~ 0.5 g of the sample (accurate to 0.001 g) into a 50 mL
polypropylene centrifuge tube, and add 20 mL of 0.15 mol/L nitric acid + 0.45 %
hydrogen peroxide solution. Make hot extraction in a thermostat at 90 ℃ for 2.5 h, and
shake for 1 min every 0.5 h. After the extraction is completed, take it out and cool it to
room temperature, and centrifuge at 8000 r/min for 15 min. Pipette the supernatant,
filter through a 0.45 μm filter membrane, and wait for determination. Do a blank test at
the same time.
NOTE. When extracting a sample, the volume of the extraction reagent (0.15 mol/L nitric acid
solution or 0.15 mol/L nitric acid + 0.45 % hydrogen peroxide solution) can be appropriately
adjusted according to the arsenic content in the sample.
19.3 Reference conditions for instruments
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
Tips & Frequently Asked QuestionsQuestion 1: How long will the true-PDF of English version of GB 5009.11-2024 be delivered?Answer: The full copy PDF of English version of GB 5009.11-2024 can be downloaded in 9 seconds, and it will also be emailed to you in 9 seconds (double mechanisms to ensure the delivery reliably), with PDF-invoice. Question 2: Can I share the purchased PDF of GB 5009.11-2024_English with my colleagues?Answer: Yes. The purchased PDF of GB 5009.11-2024_English will be deemed to be sold to your employer/organization who actually paid for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. www.ChineseStandard.us -- GB 5009.11-2024 -- Click this link and select your country/currency to pay, the exact amount in your currency will be printed on the invoice. Full PDF will also be downloaded/emailed in 9 seconds. Question 5: Should I purchase the latest version GB 5009.11-2024?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB 5009.11-2024 even if the enforcement date is in future. Complying with the latest version means that, by default, it also complies with all the earlier versions, technically. How to buy and download a true PDF of English version of GB 5009.11-2024?A step-by-step guide to download PDF of GB 5009.11-2024_EnglishStep 1: Visit website https://www.ChineseStandard.net (Pay in USD), or https://www.ChineseStandard.us (Pay in any currencies such as Euro, KRW, JPY, AUD).
Step 2: Search keyword "GB 5009.11-2024".
Step 3: Click "Add to Cart". If multiple PDFs are required, repeat steps 2 and 3 to add up to 12 PDFs to cart.
Step 4: Select payment option (Via payment agents Stripe or PayPal).
Step 5: Customize Tax Invoice -- Fill up your email etc.
Step 6: Click "Checkout".
Step 7: Make payment by credit card, PayPal, Google Pay etc. After the payment is completed and in 9 seconds, you will receive 2 emails attached with the purchased PDFs and PDF-invoice, respectively.
Step 8: Optional -- Go to download PDF.
Step 9: Optional -- Click Open/Download PDF to download PDFs and invoice.
See screenshots for above steps: Steps 1~3 Steps 4~6 Step 7 Step 8 Step 9
|