GB 5009.92-2016 (English Version) National Food Safety Standard-Determination of Calcium in Foods
Uploaded by
coolfireGB 5009.92-2016 (English Version) National Food Safety Standard-Determination of Calcium in Foods
Uploaded by
coolfirehttps://www.ChinaStandards.net -> Buy the full version pdf -> Delivered by sales@ChinaStandards.
net
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
中华人民共和国国家标准
GB 5009.92-2016
National Food Safety Standard
Determination of Calcium in Foods
食品安全国家标准
食品中钙的测定
Issued on: December 23, 2016 Implemented on: June 23, 2017
Jointly Issued by the National Health and Family Planning Commission of
the People's Republic of China and the China Food and
Drug Administration
https://www.chinastandards.net/standard/GB5009.92-2016.html
https://www.ChinaStandards.net -> Buy the full version pdf -> Delivered by [email protected]
Contents
Foreword .................................................................................................................................... i
1 Scope ................................................................................................................................... 1
2 Principle............................................................................................................................... 1
3 Reagents and Materials........................................................................................................ 1
4 Apparatuses ......................................................................................................................... 2
5 Analysis Procedures ............................................................................................................ 3
6 Expression of Analysis Results ........................................................................................... 4
7 Accuracy .............................................................................................................................. 5
8 Others .................................................................................................................................. 5
9 Principle............................................................................................................................... 5
10 Reagents and Materials...................................................................................................... 5
11 Apparatuses ....................................................................................................................... 6
12 Analysis Procedures .......................................................................................................... 6
13 Expression of Analysis Results ......................................................................................... 7
14 Accuracy ............................................................................................................................ 7
15 Others ................................................................................................................................ 8
Appendix A Reference Conditions of Temperature Programming of Microwave Digestion 9
Appendix B Reference Conditions of Flame Atomic Absorption Spectrometry ................. 10
https://www.chinastandards.net/standard/GB5009.92-2016.html
https://www.ChinaStandards.net -> Buy the full version pdf -> Delivered by [email protected]
Foreword
This standard supersedes "Determination of Calcium in Foods" (GB/T 5009.92-2003),
"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 5413.21-2010), "Determination of Copper, Iron, Zinc, Calcium, Magnesium
and Phosphorus Content in Vegetables and Derived Products" (GB/T 23375-2009),
"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 14609-2008), "Inspection of Grain and Oils - Determination of
Calcium in Cereals and Cereal Products" (GB/T 14610-2008), "Meat and Meat Products -
Method for Determination of Calcium Content" (GB/T 9695.13-2009) and "Determination
Method of Fruit Juice - Determination of Calcium and Magnesium" (NY 82.19-1988)
regarding the determination methods of calcium.
Compared with GB/T 5009.92-2003, this standard has the following main changes:
- the standard name is revised as "National Food Safety Standard - Determination of
Calcium in Foods";
- microwave digestion and pressure tank digestion are added;
- flame atomic absorption spectrometry and EDTA titrimetric method are modified;
- inductively coupled plasma atomic emission spectrometry is added;
- inductively coupled plasma mass spectrometry is added.
https://www.chinastandards.net/standard/GB5009.92-2016.html
https://www.ChinaStandards.net -> Buy the full version pdf -> Delivered by [email protected]
National Food Safety Standard
Determination of Calcium in Foods
食品安全国家标准
食品中钙的测定
1 Scope
This standard specifies flame atomic absorption spectrometry, titrimetric method,
inductively coupled plasma atomic emission spectrometry and inductively coupled plasma
mass spectrometry for the determination of calcium content in foods.
This standard is applicable to the determination of calcium content in foods.
Method I Flame Atomic Absorption Spectrometry
2 Principle
After the digestion treatment of specimen, add into lanthanum solution as the releasing
agent, and through the atomic absorption flame atomization, the absorbance value determined
at 422.7nm is in direct proportion to the calcium content within the range of certain
concentration and compare with standard series for quantitation.
3 Reagents and Materials
Unless otherwise specified, guaranteed reagents and Grade II water (defined in GB/T
6682) are adopted for the purposes of this method.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Perchloric acid (HClO4).
3.1.3 Hydrochloric acid (HCl).
3.1.4 Lanthanum oxide (La2O3).
3.2 Reagents preparation
3.2.1 Nitric acid solution (5+95): measure 50mL of nitric acid, add into 950mL of water and
mix them well.
3.2.2 Nitric acid solution (1+1): measure 500mL of nitric acid and mix it uniformly with
500mL of water.
3.2.3 Hydrochloric acid solution (1+1): measure 500mL of hydrochloric acid and mix it
https://www.chinastandards.net/standard/GB5009.92-2016.html
https://www.ChinaStandards.net -> Buy the full version pdf -> Delivered by [email protected]
uniformly with 500mL of water.
3.2.4 Lanthanum solution (20g/L): weigh 23.45g of lanthanum oxide, add into 75mL of
hydrochloric acid solution (1+1) to dissolve it after wetting it with a small amount of water,
transfer the solution to a 1 000mL volumetric flask, bring the volume to the scale with water
and then mix well.
3.3 Standards
Calcium carbonate (CaCO3, CAS No. 471-34-1): purity>99.99% or the standard calcium
solution (in certain concentration) that is approved and awarded with reference material
certificate by the nation.
3.4 Preparation of standard solution
3.4.1 Calcium standard stock solution (1 000mg/L): accurately weigh 2.496 3g (accurate to
0.000 1g) of calcium carbonate, dissolve it with hydrochloric acid solution (1+1), then
transfer it into a 1 000mL volumetric flask, bring the volume to the scale with water and mix
well.
3.4.2 Standard intermediate solution of calcium (100mg/L): accurately pipet 10mL of
calcium standard stock solution (1 000mg/L) to a 100mL volumetric flask, bring the volume
to the scale with nitric acid solution (5+95) and then mix well.
3.4.3 Standard series solution of calcium: respectively pipet 0mL, 0.500mL, 1.00mL,
2.00mL, 4.00mL and 6.00mL of standard intermediate solution of calcium (100mg/L) into
100mL volumetric flasks, add 5mL of lanthanum solution (20g/L) into each volumetric flask
and then add into nitric acid solution (5+95) to bring the volume to the scale and mix well.
The mass concentration of calcium in the standard series solution is 0mg/L, 0.500mg/L,
1.00mg/L, 2.00mg/L, 4.00mg/L and 6.00mg/L respectively.
Note: The specific concentration of elements in standard solution series may be determined according to the sensitivity of
apparatus and actual calcium content in the sample.
4 Apparatuses
Note: All the glassware and polytetrafluoroethylene digestion inner tanks shall be soaked in nitric acid solution (1+5) over
night, flushed with tap water repeatedly and finally washed clean with water.
4.1 Atomic absorption spectrometer: equipped with flame atomizer and chromium hollow
cathode lamp.
4.2 Analytical balance: with sensitivity of 1mg and 0.1mg.
4.3 Microwave digestion system: equipped with polytetrafluoroethylene digestion inner
tank.
4.4 Adjustable electrothermal furnace.
4.5 Adjustable electric hot plate.
4.6 Pressure digestion tank: equipped with polytetrafluoroethylene digestion inner tank.
4.7 Thermostatic drying oven.
4.8 Muffle furnace.
https://www.chinastandards.net/standard/GB5009.92-2016.html
https://www.ChinaStandards.net -> Buy the full version pdf -> Delivered by [email protected]
5 Analysis Procedures
5.1 Specimen preparation
Note: Specimen shall not be contaminated during the sampling and preparation processes.
5.1.1 Grain and beans samples
Pulverize the sample and store it in plastic bottle after foreign substances are removed
from it.
5.1.2 Vegetables, fruits, fish and meat samples
Clean the sample with water, dry it in the air, take the edible part to make into
homogenate and store the homogenate in the plastic bottle.
5.1.3 Such liquid sample as beverage, liquor, vinegar, soy sauce, edible oils and liquid
milk
Shake the sample well.
5.2 Specimen digestion
5.2.1 Wet digestion
Accurately weigh 0.2g~0.3g (accurate to 0.001g) of solid specimen or accurately transfer
0.500mL~5.00mL of liquid specimen to the digestion pipe with scale, add into 10mL of nitric
acid and 0.5mL of perchloric acid, digest them on adjustable electrothermal furnace
(reference conditions: 120℃/0.5h~120℃/1h, rising to 180℃/2h~180℃/4h and rising to
200℃~220℃). If the digestive solution is sepia, add into nitric acid again, digest to emit
white smoke and digestive solution acts like colorless and transparent or slightly yellow. Take
out the digestion pipe and after cooling, bring the volume to 25mL with water; dilute
according to the actual determination requirements and add certain volumes of lanthanum
solution (20g/L) into the dilute solution to make its concentration in final dilute solution be
1g/L, mix well for future use and this is the to-be-determined solution of specimen. Carry out
the reagent blank test simultaneously. Wet digestion can also be carried out on adjustable
electric hot plate with conical flask according to the above-mentioned operating methods..
5.2.2 Microwave digestion
Accurately weigh 0.2g~0.8g (accurate to 0.001g) of solid specimen or accurately transfer
0.500mL~3.00mL of liquid specimen into the microwave digestion tank, add into 5mL of
nitric acid, and digest the specimen according to the operation procedures of microwave
digestion (see Appendix A for digestion conditions). After cooling, take out the digestion tank,
and catch acid to about 1mL by placing it on 140℃~160℃ electric hot plate. After the
digestion tank cools down, transfer the digestive solution to a 25mL volumetric flask, wash
the digestion tank for 2~3 times with a small amount of water, combine the washing solution
to the volumetric flask and bring the volume to the scale with water. Dilute according to the
actual determination requirements and add certain volumes of lanthanum solution (20g/L)
into the dilute solution to make its concentration in final dilute solution be 1g/L, mix well for
future use and this is the to-be-determined solution of specimen. Carry out the reagent blank
test simultaneously.
5.2.3 Pressure tank digestion
Accurately weigh 0.2g~1g (accurate to 0.001g) of solid specimen or accurately transfer
0.500mL~5.00mL of liquid specimen into the digestion inner tank and add into 5mL of nitric
https://www.chinastandards.net/standard/GB5009.92-2016.html
