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GB 5009.13-2017 English PDF (GB5009.13-2017)

GB 5009.13-2017 English PDF (GB5009.13-2017)

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GB 5009.13-2017: National food safety standard -- Determination of copper in foods

This standard specifies the determination of copper content in food by graphite furnace and flame atomic absorption spectrometry, inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission spectrometry.
GB 5009.13-2017
GB
NATIONAL STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
National food safety standard -
Determination of copper in foods
ISSUED ON. APRIL 06, 2017
IMPLEMENTED ON. OCTOBER 06, 2017
Issued by. National Health and Family Planning Commission of the PRC;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 5
5 Analytical procedures ... 6
6 Presentation of analytical results ... 8
7 Precision... 9
8 Others ... 9
9 Principle... 9
10 Reagents and materials... 10
11 Instruments and equipment ... 11
12 Analytical procedures ... 11
13 Presentation of analytical results ... 12
14 Precision ... 13
15 Others ... 13
Appendix A Microwave digestion temperature rising program ... 14
Appendix B Instrument reference conditions of graphite furnace atomic
absorption spectrometry ... 15
Appendix C Flame atomic absorption spectrometry instrument reference
conditions ... 16
Foreword
This standard replaces GB/T 5009.13-2003 ?€?Determination of copper in food?€?, GB 5413.21-2010 ?€?National food safety standard - Determination of calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese in foods for infants and young children, milk and milk products?€?, GB/T 23375-2009
?€?Determination of copper, iron, zinc, calcium, magnesium and phosphorus content in vegetables and derived products?€?, GB/T 9695.22-2009 ?€?Meat and meat products - Determination of copper content?€?, GB/T 14609-2008
?€?Inspection of grain and oils?€?Determination of copper, iron, manganese, zinc, calcium, magnesium in cereals and derived products by atomic absorption and flame spectrophotometry?€?, GB/T 18932.12-2002 ?€?Method for the determination of potassium, sodium, calcium, magnesium, zinc, iron, copper, manganese, chromium, lead, cadmium contents in honey - Atomic absorption spectrometry?€?, and NY/T 1201-2006 ?€?Determination of copper iron and zinc content in
vegetables and derived products?€?.
As compared with GB/T 5009.13-2003, the main changes of this standard are as follows.
- CHANGE the standard name into ?€?National food safety standard -
Determination of copper in foods?€?;
- In the pretreatment method, ADD the wet digestion, pressure tank
digestion, and microwave digestion;
- RETAIN the graphite furnace atomic absorption spectrometry method as
the first method, using the ammonium dihydrogen phosphate-palladium
nitrate solution as a matrix modifier; RETAIN the flame atomic absorption spectrometry method as the second method; and DELETE the
diethyldithiocarbamate colorimetric method
- ADD the inductively coupled plasma mass spectrometry method as the
third method;
- ADD the inductively coupled plasma emission spectrometry method as the fourth method;
- ADD the microwave digestion temperature rising program, graphite
furnace atomic absorption spectrometry and flame atomic absorption
spectrometry instrument reference conditions as the appendixes.
National food safety standard -
Determination of copper in foods
1 Scope
This standard specifies the determination of copper content in food by graphite furnace and flame atomic absorption spectrometry, inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission
spectrometry.
This standard applies to the determination of copper in all types of foods. Method 1. Graphite furnace atomic absorption spectrometry
2 Principle
After digestion, the sample is atomized in graphite furnace AND the
absorbance is measured at 324.8 nm. In a certain concentration range, the copper absorbance value is proportional to the copper content, AND it is compared with the standard series for quantitative.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are excellent pure AND the water is the level 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].
3.2 Reagent preparation
3.2.1 Nitric acid solution (5 + 95). MEASURE 50 mL of nitric acid; slowly ADD it into 950 mL of water; MIX it uniformly.
3.2.2 Nitric acid solution (1 + 1). MEASURE 250 mL of nitric acid; slowly ADD it into 250 mL of water; MIX it uniformly.
3.2.3 Ammonium dihydrogen phosphate-palladium nitrate solution. WEIGH
0.02 g of palladium nitrate; ADD a small amount of nitric acid solution (1 + 1) to dissolve it; ADD 2 g of ammonium dihydrogen phosphate; after dissolving, USE the nitric acid solution (5 + 95) to make its volume reach to 100 mL; MIX it uniformly.
3.3 Standard substance
Copper sulfate pentahydrate (CuSO4 ?€? 5H2O, CAS No.. 7758-99-8). purity > 99.99%, OR the copper standard solution of a certain concentration certified and awarded with the standard substance certificate by the state.
3.4 Standard solution preparation
3.4.1 Standard copper stock solution (1000 mg/L). Accurately WEIGH 3.9289 g (accurate to 0.0001 g) of copper sulfate pentahydrate; USE a small amount of nitric acid (1 + 1) to dissolve it; TRANSFER t into a 1000 mL volumetric flask; ADD water to the mark; MIX it uniformly.
3.4.2 Copper standard intermediate solution (1.00 mg/L). Accurately PIPETTE 1.00 mL of copper standard stock solution (1000 mg/L) into a 1000 mL
volumetric flask; ADD nitric acid solution (5 + 95) to the mark; MIX it uniformly. 3.4.3 Copper standard series solution. respectively PIPETTE 0 mL, 0.500 mL, 1.00 mL, 2.00 mL, 3.00 mL and 4.00 mL of copper standard intermediate
solution (1.00 mg/L) into a 100 mL volumetric flask; ADD nitric acid solution (5 + 95) to the mark; MIX it uniformly. The concentration of this copper standard series solution is 0 ??g/L, 5.00 ??g/L, 10.0 ??g/L, 20.0 ??g/L, 30.0 ??g/L and 40.0 ??g/L, respectively.
Note. It may be based on the sensitivity of the instrument and the actual content of copper in the sample to determine the mass concentration of the copper element in the standard series solution.
4 Instruments and equipment
Note. All glassware and Teflon digestion inner tanks must be soaked in nitric acid (1 + 5) overnight, rinsed repeatedly with tap water, and finally rinsed clean with water.
4.1 Atomic absorption spectrometer. with graphite furnace atomizer and
copper hollow cathode lamp.
4.2 Analytical balance. sensitivity of 0.1 mg and 1 mg.
4.3 Adjustable electric furnace.
4.4 Adjustable heating plate.
4.5 Microwave digestion system. with polytetrafluoroethylene digestion inner tank.
4.6 Pressure digestion tank. with polytetrafluoroethylene digestion inner tank. 4.7 Constant temperature drying oven.
4.8 Muffle furnace.
5 Analytical procedures
5.1 Sample preparation
Note. Sample contamination shall be avoided during sampling and sample
preparation.
5.1.1 Food and beans samples
After removing of debris, the sample is crushed and stored in a plastic bottle. 5.1.2 Vegetables, fruits, fish, meat and other samples
The sample is washed with water and dried naturally, AND the edible part is taken to be homogenized and stored in plastic bottles.
5.1.3 Drinks, wine, vinegar, soy sauce, edible vegetable oil, liquid milk and other liquid samples
SHAKE the sample uniformly.
5.2 Sample preparation
5.2.1 Wet digestion
WEIGH 0.2 g ~ 3 g (accurate to 0.001 g) of solid sample or accurately
PIPETTE 0.500 mL ~ 5.00 mL of liquid sample into in the graduated digestion tube; ADD 10 mL of nitric acid and 0.5 mL of perchloric acid; MAKE it digested on the adjustable electric furnace (reference conditions. 120 ??C / 0.5 h ~ 1 h; rise the temperature to 180 ??C / 2 h ~ 4 h; rise the temperature to 200 ??C ~ 220 ??C). If the digestion solution is in tan, ADD a small amount of nitric acid to digest it until white smoke is produced and the digestion solution is in colorless transparent or slightly yellow; TAKE the digestion tube out; COOL it down, USE water to make its volume reach to 10 mL; MIX it uniformly to prepare for use. Meanwhile MAKE the reagent blank test. It may also use the conical flask; and PERFORM wet digestion on the adjustable heating plate in accordance with the aforementioned operation procedures.
5.2.2 Microwave digestion...

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