GB 5009.92-2016 PDF English
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Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
GB 5009.92-2016 | English | 70 |
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National food safety standard - Determination of calcium in foods
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GB/T 5009.92-2003 | English | 239 |
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Determination of calcium in foods
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GB 5009.92-2016: National food safety standard - Determination of calcium in foods---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/GB5009.92-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of calcium in foods
Issued on. DECEMBER 23, 2016
Implemented on. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China;
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 Analysis procedure... 6
6 Expression of analysis results... 8
7 Precision... 9
8 Others... 9
9 Principle... 9
10 Reagents and materials... 9
11 Instruments and equipment... 10
12 Analysis procedure... 10
13 Expression of analysis results... 11
14 Precision... 12
15 Others... 12
Annex A Microwave digestion temperature rise program reference conditions... 13
Annex B Flame atomic absorption spectrometry reference conditions... 14
Foreword
This Standard replaces the determination method for calcium in GB/T 5009.92-2003
“Determination of calcium in foods”, 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 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 14610-2008 “Inspection of grain and oils - Determination of
calcium in cereals and cereal products”, GB/T 9695.13-2009 “Meat and meat products
- Method for Determination of calcium content” and NY 82.19-1988 “Determination of
fruit juice - Determination of calcium and magnesium”.
Compare this Standard with GB/T 5009.92-2003, the main changes are as follows.
- MODIFY the standard name TO "National food safety standard - Determination of
calcium in foods";
- ADD the microwave digestion, pressure tank digestion;
- MODIFY the flame atomic absorption spectrometry and EDTA titration;
- ADD the inductively coupled plasma emission spectrometry;
- ADD the inductively coupled plasma mass spectrometry.
National food safety standard -
Determination of calcium in foods
1 Scope
This Standard specifies the determination of calcium in foods by flame atomic
absorption spectrometry, titration, inductively coupled plasma atomic emission
spectrometry and inductively coupled plasma mass spectrometry.
This Standard applies to the determination of calcium content in foods.
Method 1 -- Flame atomic absorption spectrometry
2 Principle
After the sample is digested, add lanthanum solution as the releasing agent, atomize
by atomic absorption flame, and measure the absorbance value at 422.7 nm, which is
proportional to the calcium content in a certain concentration range. Compare with the
standard series.
3 Reagents and materials
Unless otherwise specified, the reagents used in this method are excellent regents,
and the water is Grade 2 water as specified in GB/T 6682.
3.1 Reagents
3.2 Preparation of reagents
3.2.1 Nitric acid solution (5 + 95). MEASURE 50 mL of nitric acid; ADD 950 mL of water;
MIX well.
3.3 Standard
Calcium carbonate (CaCO3, CAS No. 471-34-1). Purity > 99.99 %, or calcium standard
solution at a certain concentration certified by the state and awarded the standard
substance certificate.
3.4 Preparation of standard solutions
3.4.1 Calcium standard stock solution (1000 mg/L). accurately WEIGH 2.4963 g (to
the nearest 0.0001 g) of calcium carbonate; ADD hydrochloric acid solution (1 + 1) to
dissolve; TRANSFER to a 1000 mL volumetric flask; ADD water to the mark; MIX well.
4 Instruments and equipment
NOTE. All glassware and polytetrafluoroethylene digestion inner tank must be soaked in nitric
acid solution (1 + 5) overnight, washed repeatedly with tap water, and finally rinsed with water.
4.1 Atomic absorption spectrometer. with flame atomizer, calcium hollow cathode lamp.
4.4 Adjustable electric furnace.
4.5 Adjustable electric hot plate.
4.6 Pressure digestion tank. with polytetrafluoroethylene digestion inner tank.
4.7 Constant temperature oven.
5 Analysis procedure
5.1 Sample preparation
NOTE. Sample contamination shall be avoided during sampling and sample preparation
processes.
5.2 Sample digestion
5.2.1 Wet digestion
Accurately WEIGH 0.2 g ~ 3 g (to the nearest 0.001 g) of solid sample or accurately
PIPETTE 0.500 mL ~ 5.00 mL of liquid sample in a graduated digestion tube;
5.2.2 Microwave digestion
Accurately WEIGH 0.2 g ~ 3 g (to the nearest 0.001 g) of solid sample or accurately
PIPETTE 0.500 mL ~ 3.00 mL of liquid sample in a microwave digestion tank; ADD 5
mL of nitric acid. DIGEST the sample according to procedure of the microwave
digestion, refer to Annex A for digestion conditions. REMOVE the digestion tank after
cooling; PLACE it on the electric hot plate to get rid of acid to about 1 mL at 140 °C ~
160 °C. After the digestion tank is cool, TRANSFER the digestion solution to a 25 mL
volumetric flask;
5.3 Instrument reference conditions
See Annex B for reference conditions.
5.4 Plotting of standard curve
The calcium standard series solutions are introduced into the flame atomizer according
to the order of the concentration from low to high, the absorbance values are measured.
The standard curve is plotted by taking the concentration of calcium in the standard
series solutions as the abscissa and the corresponding absorbance values as the
ordinate.
6 Expression of analysis results
The content of calcium in the sample is calculated according to equation (1).
7 Precision
The absolute difference between two independent determination results obtained
under repeatability conditions shall not exceed 10 % of the arithmetic mean.
8 Others
When weighing 4 g (or 4 mL) of sample, diluting to the constant volume of 25 mL for
calculation,
9 Principle
Within the proper pH range, calcium forms metal complex with EDTA (disodium
ethylenediaminetetraacetate).
10 Reagents and materials
Unless otherwise specified, the reagents used in this method are analytical regents,
and the water is Grade 3 water as specified in GB/T 6682.
10.1 Reagents
10.1.6 Calcium red indicator (C21O7N2SH14).
10.1.7 Nitric acid (HNO3). excellent regent.
10.1.8 Perchloric acid (HClO4). excellent regent.
10.2 Preparation of reagents
10.2.1 Potassium hydroxide solution (1.25 mol/L). WEIGH 70.13 g of potassium
hydroxide; DILUTE with water to 1000 mL; MIX well.
10.2.6 Hydrochloric acid solution (1 + 1). MEASURE 500 mL of hydrochloric acid; MIX
well with 500 mL of water.
10.3 Standard
Calcium carbonate (CaCO3, CAS No. 471-34-1). with purity > 99.99 %, or calcium
standard solution at a certain concentration certified by the state and awarded the
standard substance certificate.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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