GB 5009.13-2017_English: PDF (GB5009.13-2017)
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National food safety standard -- Determination of copper in foods
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GB 5009.13-2017
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| GB/T 5009.13-2003 | English | 239 |
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Determination of copper in foods
| Obsolete |
GB/T 5009.13-2003
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| GB/T 5009.13-1996 | English | 199 |
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Method for determination of copper in foods
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GB/T 5009.13-1996
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| GB 5009.13-1985 | English | 199 |
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Method for determination of copper in foods
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GB 5009.13-1985
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| Standard ID | GB 5009.13-2017 (GB5009.13-2017) | | Description (Translated English) | National food safety standard -- Determination of copper in foods | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 12,119 | | Date of Issue | 2017-04-06 | | Date of Implementation | 2017-10-06 | | Older Standard (superseded by this standard) | GB/T 23375-2009 Partial; GB/T 9695.22-2009; GB/T 14609-2008 Partial; GB/T 5009.13-2003; GB/T 18932.12-2002 Partial; GB 5413.21-2010 Partial; NY/T 1201-2006 Partial | | Regulation (derived from) | State Health and Family Planning Commission Notice No. 5 of 2017 | | Standard ID | GB/T 5009.13-2003 (GB/T5009.13-2003) | | Description (Translated English) | Determination of copper in foods | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.040 | | Word Count Estimation | 6,611 | | Date of Issue | 2003-08-11 | | Date of Implementation | 2004-01-01 | | Older Standard (superseded by this standard) | GB/T 5009.13-1996 | | Quoted Standard | GB/T 5009.11-2003; | | Drafting Organization | Ministry of Health Food Hygiene Supervision and Inspection | | Administrative Organization | People's Republic of China Ministry of Health | | Summary | This standard specifies: copper in foods Determination. This standard applies to: copper in foods Determination. The detection limit of this method | | Standard ID | GB/T 5009.13-1996 (GB/T5009.13-1996) | | Description (Translated English) | Method for determination of copper in foods | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.04 | | Word Count Estimation | 4,459 | | Date of Issue | 1996/6/19 | | Date of Implementation | 1996/9/1 | | Older Standard (superseded by this standard) | GB 5009.13-1985 |
GB 5009.13-2017
GB
NATIONAL STANDARD
OF THE PEOPLE’S 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 μg/L, 5.00 μg/L, 10.0 μg/L, 20.0 μg/L, 30.0 μg/L and 40.0
μg/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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