GB 5009.76-2014 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.76-2014 | English | 85 |
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National food safety standard - Determination of arsenic in food Additives
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| GB/T 5009.76-2003 | English | 279 |
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Determination of arsenic in food additives
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GB 5009.76-2014: National food safety standard - Determination of arsenic in food Additives---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/GB5009.76-2014
GB
NATIONAL STANDARD
National food safety standard -
Determination of arsenic in food additives
Issued on. SEPTEMBER 21, 2015
Implemented on. MARCH 21, 2016
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword... 3
1 Scope... 4
2 Principles... 4
3 Reagents and materials... 4
4 Instruments... 6
5 Sample treatment... 8
6 Determination... 9
7 Expression of analytical results... 10
8 Precision... 11
9 Principles... 11
10 Reagent... 11
11 Instruments... 13
12 Analytical procedures... 13
13 Expression of analytical results... 15
14 Precision... 15
15 Others... 16
Foreword
This standard replaces GB/T 5009.76-2003 “Determination of arsenic in food
additives”.
As compared with GB/T 5009.76-2003, the main changes of this standard are
as follows.
- CHANGE the standard name into “National food safety standard –
Determination of arsenic in food additives”;
- DELETE the arsenic spot method;
- ADD the hydride atomic fluorescence determination method, as the
method 2.
National food safety standard -
Determination of arsenic in food additives
1 Scope
This standard specifies the determination of arsenic in food additives.
This standard applies to the determination of arsenic in food additives.
Method 1.Diethylamino dithiocarbamate colorimetric method
2 Principles
In the presence of potassium iodide and stannous chloride, the high valence
arsenic in the sample solution is reduced to trivalent arsenic, AND the trivalent
arsenic reacts with the newly generated hydrogen which is produced by the
zinc particles and acid, to produce arsine gas;
3 Reagents and materials
Note. Unless otherwise stated, the reagents used in this method are of
analytical pure AND the water is level 1 water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3). excellent grade pure.
3.1.11 Pyridine (C5H5N).
3.1.12 Silver diethyldithiocarbamate (C5H10AgNS2).
3.1.13 Triethanolamine (C6H15NO3).
3.1.14 Ethanol (C2H5OH).
3.1.15 Phenolphthalein (C2OH14O4).
3.1.16 Lead acetate (C4H6O4Pb • H2O).
3.2 Reagent preparation
3.2.1 Sulfuric acid solution (1 + 1). MEASURE 100 mL of sulfuric acid; slowly
ADD it into 100 mL of water; MIX it uniformly; COOL it down before use.
3.2.2 Sulfuric acid solution (1 mol/L). MEASURE 28 mL of sulfuric acid; slowly
ADD it into water; USE water to dilute it to 500 mL.
3.2.3 Hydrochloric acid solution (1 + 1). MEASURE 100 mL of hydrochloric
acid; slowly ADD it into 100 mL of water; MIX it uniformly; COOL it down before
use.
3.2.10 Phenolphthalein ethanol solution (10 g/L). WEIGH 1.0 g of
phenolphthalein; DISSOLVE it into 100 mL of ethanol solution.
3.2.11 Lead acetate solution (100 g/L). WEIGH 10 g of lead acetate; USE
water to dissolve it and MAKE its volume reach to 100 mL.
3.3 Standard substance
Arsenic trioxide (As2O3) standard substance. the purity is 99.99% OR the
standard substance certified and awarded the standard substance certificate
by the state.
3.4 Standard solution preparation
3.5 Materials
Lead acetate cotton. DIP the absorbent cotton into the lead acetate solution
(10%) for 2 h; TAKE it out and DRY it naturally.
4 Instruments
Note. The glass instruments used shall be soaked in the nitric acid solution (1
+ 4) for more than 24 h; USE water to rinse it for several times; USE deionized
water to rinse it clean.
4.1 Spectrophotometer.
4.5 Electric heating plate.
4.6 Arsenic determination device (SEE Figure 1).
5 Sample treatment
5.1 Preparation of inorganic samples
The “sample treatment” of the inorganic sample may be carried out in
accordance with the method as specified in the relevant standards.
5.2 Preparation of organic samples
The “sample treatment” of organic sample shall, in addition to the requirements
of relevant standards, generally follow the methods below.
6 Determination
6.1 Selection of absorption solution
The absorption solution A or the absorption solution B can be selected in
accordance with the demands of analysis. During the determination process,
the same absorption solution is applied to the sample, blank and standard
solution.
6.2 Limited amount test
6.2.1 PIPETTE a certain amount of sample solution and arsenic standard use
solution (arsenic content of not less than 5 μg), respectively, into the arsenic
generation bottle A; ADD sulfuric acid to a total of 5 mL; ADD 50 mL of water.
6.2.2 In each bottle as mentioned in 6.2.1, ADD 3 mL of potassium iodide
solution; MIX it uniformly; LET it stand for 5 min.
6.2.3 USE the visual colorimetric method or USE the 1 cm cuvette to
determine the absorbance of the absorption solution at the wavelength 515 nm
(absorption solution A) or the wavelength 540 nm (absorption solution B).
6.3 Quantitative determination
6.3.1 PIPETTE 25 mL (or the appropriate amount of) sample solution and the
same amount of reagent blank solution; respectively PLACE it into the arsenic
generation bottle A; ADD sulfuric acid to a total of 5 mL; ADD 50 mL of water.
6.3.3 ADD 3 mL of potassium iodide solution into the sample solution, reagent
blank solution and arsenic standard solution; MIX it uniformly; LET it stand for
5 min; then respectively ADD 1 mL of stannous chloride solution; MIX it
uniformly; LET it stand for 15 min; respectively ADD 5 g arsenic-free metal zinc;
immediately PLUG the air duct B which is equipped with the lead acetate
cotton lead, to make the tip of the air duct B insert into the absorption tube C
which contains 5.0 mL of absorption solution A or absorption solution B;
7 Expression of analytical results
Arsenic content in the sample is calculated in accordance with the formula (1).
8 Precision
The absolute difference between the two independent determinations obtained
under repeatability shall not exceed 10% of the arithmetic mean.
9 Principles
After digestion of the sample, thiourea is added to reduce the pentavalent
arsenic to trivalent arsenic, AND then the sodium borohydride or potassium
borohydride is added to reduce it into arsine, which is carried by the argon into
the quartz atomizer to be decomposed into atomic arsenic. It produces atomic
fluorescence under the excitation of the emitted light from the special arsenic
hollow cathode,
10 Reagent
Note. Unless otherwise stated, the reagents used in this method are of
analytical pure AND the water is level 1 water as specified in GB/T 6682.
10.1 Reagents
10.1.10 Hydrogen peroxide (H2O2).
10.2 Reagent preparation
10.2.1 Sodium hydroxide solution (2 g/L). WEIGH 2.0 g of sodium hydroxide;
DISSOLVE it into 1000 mL of water; MIX it uniformly.
10.2.2 Sodium borohydride solution (10 g/L). WEIGH 10.0 g of sodium
borohydride; DISSOLVE it into 1000 mL of sodium hydroxide solution; MIX it
uniformly. PREPARE it before use (it may also weigh 14 g of potassium
borohydride to substitute sodium borohydride).
10.3 Standard substance
Arsenic trioxide (As2O3) standard substance. the purity is 99.99% OR the
standard substance certified and awarded the standard substance certificate
by the state.
10.4 Standard solution preparation
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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