GB 1903.63-2023 English PDF

GB 1903.63-2023: National food safety standard - Food nutritional fortification - Calcium glycerophosphate
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GB 1903.63-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Nutritional Enhancer
- Calcium Glycerophosphate
ISSUED ON: SEPTEMBER 06, 2023
IMPLEMENTED ON: MARCH 06, 2024
Issued by: National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
2 Chemical name, molecular formula, structural formula and relative molecular mass3
3 Technical requirements ... 3
Annex A Inspection methods ... 5
Annex B Standard infrared spectrum of calcium glycerophosphate ... 13
National Food Safety Standard - Food Nutritional Enhancer
- Calcium Glycerophosphate
1 Scope
This Standard applies to calcium glycerophosphate, the food nutritional enhancer
obtained by neutralizing glycerophosphate with calcium hydroxide or calcium
carbonate.
2 Chemical name, molecular formula, structural formula and
relative molecular mass
2.1 Chemical name
Calcium glycerophosphate
2.2 Molecular formula
C3H7CaO6P
2.3 Structural formula
2.4 Relative molecular mass
210.14 (according to the 2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall comply with the requirements in Table 1.
Annex A
Inspection methods
A.1 General
The reagents and water used in this standard refer to analytically pure reagents and
grade 3 water specified in GB/T 6682 unless otherwise specified. Standard solutions,
standard solutions for impurity determination, preparations and products used in the test
are prepared in accordance with the provisions of GB/T 601, GB/T602 and GB/T603
unless otherwise specified. Solutions used in the test refer to aqueous solutions unless
otherwise specified.
A.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Nitric acid.
A.2.1.2 Molybdic acid.
A.2.1.3 Ammonia water.
A.2.1.4 Hydrochloric acid solution: 3.65 g/L.
A.2.1.5 Dilute nitric acid solution: Take 105 mL of nitric acid (A.2.1.1) and dilute to
1000 mL with water.
A.2.1.6 Ammonium molybdate solution: Weigh 6.5 g of molybdic acid (A.2.1.2). Add
14 mL of water and 14.5 mL of ammonia water (A.2.1.3). Shake to dissolve. Cool.
While stirring, slowly add to a mixture of 32 mL of cooled dilute nitric acid solution
(A.2.1.5) and 40 mL of water. Let stand for 48 h. Filter. Take the filtrate.
A.2.2 Instruments and equipment
A.2.2.1 Balance: sensitivity is 0.001 g.
A.2.2.2 Platinum wire: 1 piece.
A.2.3 Identification methods
A.2.3.1 Solubility test
Weigh about 1.0 g of the specimen. Add 10 mL of water ≤5°C to dissolve. Boil. White
crystals will precipitate.
A.2.3.2 Identification of ammonium molybdate
Weigh 0.1 g (accurate to 0.001 g) of the specimen. Dissolve it in 10 mL of water and
10 mL of dilute nitric acid solution (A.2.1.5). Add 5 mL of ammonium molybdate
solution (A.2.1.6). Boil until a yellow precipitate is produced.
A.2.3.3 Identification of calcium
Take a platinum wire. Wet it with hydrochloric acid solution (A.2.1.4), and dip it into
the specimen to take sample. Burn it in a colorless flame, and the flame will appear
brick red.
A.2.3.4 Infrared identification
Take an appropriate amount of dry sample. Place it in an agate mortar and grind it evenly.
Put it into a mold, press it tightly and scan it. The infrared spectrum of the sample shall
be consistent with the infrared spectrum of the calcium glycerophosphate standard.
Refer to Figure B.1 in Annex B for the infrared spectrum of the calcium
glycerophosphate standard.
A.3 Determination of calcium glycerophosphate content (on a dry basis)
A.3.1 Method summary
In the test solution, calcium carboxylic acid is used as an indicator and titrated with
EDTA-2Na standard titration solution. The content is calculated based on the amount
of EDTA-2Na standard titration solution consumed.
A.3.2 Reagents and materials
A.3.2.1 Sodium chloride.
A.3.2.2 Calcium carboxylate indicator.
A.3.2.3 Sodium hydroxide.
A.3.2.4 Calcium indicator: Weigh 10 g of sodium chloride (A.3.2.1) that has been dried
at 105℃~110℃ for 2 h. Grind it into a fine powder in a mortar. Then add 0.1 g of
calcium carboxylate indicator (A.3.2.2). Grind it into a fine powder. Mix well.
A.3.2.5 Hydrochloric acid solution (1+1): Add concentrated hydrochloric acid to an
equal volume of water.
A.3.2.6 Sodium hydroxide solution (10 mol/L): Weigh 400 g of sodium hydroxide
(A.3.2.3) and dilute to 1000 mL with water.
A.3.2.7 Disodium ethylenediaminetetraacetic acid standard titration solution: c (EDTA)
= 0.05 mol/L.
A.3.3 Instruments and equipment
A.5.2 Instruments and equipment
Balance: sensitivity is 0.0001 g.
A.5.3 Analysis steps
Weigh 1 g of the specimen (accurate to 0.0001 g). Place it in 100 mL of carbon dioxide-
free water. Add 2 drops of phenolphthalein indicator (A.5.1.7). If the solution is pink,
add hydrochloric acid solution (A.5.1.5) until it is colorless. Record the volume of
hydrochloric acid solution (A.5.1.5) added. If the solution is colorless, add sodium
hydroxide solution (A.5.1.6) until the solution is pink. Record the volume of sodium
hydroxide added.
A.5.4 Calculation of results
The volume of hydrochloric acid or sodium hydroxide consumed in titration per gram
of sample is taken as the measurement result.
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 10% of the arithmetic mean.
A.6 Free glycerol and alcohol-soluble substances
A.6.1 Reagents and materials
Absolute ethanol.
A.6.2 Instruments and equipment
A.6.2.1 Balance: sensitivity 0.0001 g.
A.6.2.2 Constant temperature drying oven: accuracy is 70℃±2℃.
A.6.2.3 Constant temperature water bath.
A.6.3 Analysis steps
Weigh 1 g of the specimen (accurate to 0.0001 g). Add 25 mL of anhydrous ethanol.
Shake for 2 min. Filter. Wash the residue with 5 mL of anhydrous ethanol. Combine the
filtrate and washings. Evaporate to dryness on a water bath. Place in a constant
temperature drying oven. Dry the residue at 70℃±2℃ for 1 h.
A.6.4 Result calculation
The mass fraction w3 of free glycerol and alcohol-soluble matter in calcium
glycerophosphate is calculated according to formula (A.3).
Where,
m - Mass of the residue after drying, in grams (g);
m0 - Mass of the specimen, in grams (g);
The calculation result is expressed to 1 decimal place.
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 0.5% of the arithmetic mean.
A.7 Determination of phosphate
A.7.1 Reagents and materials
A.7.1.1 Nitric acid.
A.7.1.2 Molybdic acid.
A.7.1.3 Ammonia water.
A.7.1.4 Potassium dihydrogen phosphate.
A.7.1.5 Dilute nitric acid solution: Take 105 mL of nitric acid (A.7.1.1). Dilute it to
1000 mL with water.
A.7.1.6 Ammonium molybdate solution: Weigh 6.5 g of molybdic acid (A.7.1.2). Add
14 mL of water and 14.5 mL of ammonia water (A.7.1.3). Shake to dissolve. Cool.
While stirring, slowly add to the cooled mixture of 32 mL of nitric acid (A.7.1.1) and
40 mL of water. Let stand for 48 h. Filter. Take the filtrate.
A.7.1.7 Phosphate standard stock solution: Accurately weigh 0.192 g of potassium
dihydrogen phosphate (A.7.1.4). Dilute to 100 mL with water.
A.7.1.8 Phosphate standard working solution: Pipette 3 mL of phosphate standard stock
solution (A.7.1.7). Add dilute nitric acid solution (A.7.1.5) to 100 mL.
A.7.2 Instruments and equipment
Balance: sensitivity is 0.0001 g.
A.7.3 Analysis steps
Weigh 1 g of the specimen (accurate to 0.0001 g). Place in a 25 mL Nessler colorimetric
tube. Add 10 mL of dilute nitric acid solution (A.7.1.5) to dissolve. Add 10 mL of
ammonium molybdate solution (A.7.1.6). Shake well. Let stand for 10 min. Compare
with the control solution made from 10 mL of phosphate standard working solution
(A.7.1.8). The turbidity of the sample solution is not darker than that of the standard
solution, that is, the phosphate content in the sample is ≤0.04%.
A.8 Determination of sulfate
A.8.1 Reagents and materials
A.8.1.1 Potassium sulfate.
A.8.1.2 Acetic acid.
A.8.1.3 Barium chloride.
A.8.1.4 Acetic acid solution: Take 30 mL of acetic acid (A.8.1.2). Dilute to 100 mL with
water.
A.8.1.5 Barium chloride solution: Weigh 25 g of barium chloride (A.8.1.3). Dissolve it
in a small amount of water and make up to 100 mL.
A.8.1.6 Sulfate standard solution: Weigh 0.181 g (accurate to 0.0001 g) of potassium
sulfate (A.8.1.1). Dissolve it in an appropriate amount of water. Dilute to 1000 mL.
A.8.2 Instruments and equipment
Balance: sensitivity is 0.0001 g.
A.8.3 Analysis steps
Weigh 0.5 g of the specimen (accurate to 0.0001 g) and place it in a 25 mL Nessler
colorimetric tube. Add water to dissolve to 15 mL (a small amount of acetic acid can be
added to increase the solubility). At the same time, draw 5.0 mL of sulfate standard
solution (A.8.1.6) into another Nessler colorimetric tube. Add 0.5 mL of acetic acid
solution (A.8.1.4) and 1 mL of barium chloride solution (A.8.1.5) to each of them. Place
the colorimetric tubes with sulfate standard solution and test solution in a backlit place.
Let them stand for 5 min. Under the condition of a black background, observe and
compare from top to bottom. The turbidity of the specimen solution is not darker than
that of the standard solution, that is, the sulfate content in the specimen is ≤0.1%.
A.9 Determination of chloride
A.9.1 Reagents and materials
A.9.1.1 Sodium chloride.
A.9.1.2 Acetic acid.
A.9.1.3 Nitric acid.
A.9.1.4 Silver nitrate.
A.9.1.5 Acetic acid solution: Take 30 mL of acetic acid (A.9.1.2) and dilute to 100 mL
with water.
GB 1903.63-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Nutritional Enhancer
- Calcium Glycerophosphate
ISSUED ON: SEPTEMBER 06, 2023
IMPLEMENTED ON: MARCH 06, 2024
Issued by: National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
2 Chemical name, molecular formula, structural formula and relative molecular mass3
3 Technical requirements ... 3
Annex A Inspection methods ... 5
Annex B Standard infrared spectrum of calcium glycerophosphate ... 13
National Food Safety Standard - Food Nutritional Enhancer
- Calcium Glycerophosphate
1 Scope
This Standard applies to calcium glycerophosphate, the food nutritional enhancer
obtained by neutralizing glycerophosphate with calcium hydroxide or calcium
carbonate.
2 Chemical name, molecular formula, structural formula and
relative molecular mass
2.1 Chemical name
Calcium glycerophosphate
2.2 Molecular formula
C3H7CaO6P
2.3 Structural formula
2.4 Relative molecular mass
210.14 (according to the 2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall comply with the requirements in Table 1.
Annex A
Inspection methods
A.1 General
The reagents and water used in this standard refer to analytically pure reagents and
grade 3 water specified in GB/T 6682 unless otherwise specified. Standard solutions,
standard solutions for impurity determination, preparations and products used in the test
are prepared in accordance with the provisions of GB/T 601, GB/T602 and GB/T603
unless otherwise specified. Solutions used in the test refer to aqueous solutions unless
otherwise specified.
A.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Nitric acid.
A.2.1.2 Molybdic acid.
A.2.1.3 Ammonia water.
A.2.1.4 Hydrochloric acid solution: 3.65 g/L.
A.2.1.5 Dilute nitric acid solution: Take 105 mL of nitric acid (A.2.1.1) and dilute to
1000 mL with water.
A.2.1.6 Ammonium molybdate solution: Weigh 6.5 g of molybdic acid (A.2.1.2). Add
14 mL of water and 14.5 mL of ammonia water (A.2.1.3). Shake to dissolve. Cool.
While stirring, slowly add to a mixture of 32 mL of cooled dilute nitric acid solution
(A.2.1.5) and 40 mL of water. Let stand for 48 h. Filter. Take the filtrate.
A.2.2 Instruments and equipment
A.2.2.1 Balance: sensitivity is 0.001 g.
A.2.2.2 Platinum wire: 1 piece.
A.2.3 Identification methods
A.2.3.1 Solubility test
Weigh about 1.0 g of the specimen. Add 10 mL of water ≤5°C to dissolve. Boil. White
crystals will precipitate.
A.2.3.2 Identification of ammonium molybdate
Weigh 0.1 g (accurate to 0.001 g) of the specimen. Dissolve it in 10 mL of water and
10 mL of dilute nitric acid solution (A.2.1.5). Add 5 mL of ammonium molybdate
solution (A.2.1.6). Boil until a yellow precipitate is produced.
A.2.3.3 Identification of calcium
Take a platinum wire. Wet it with hydrochloric acid solution (A.2.1.4), and dip it into
the specimen to take sample. Burn it in a colorless flame, and the flame will appear
brick red.
A.2.3.4 Infrared identification
Take an appropriate amount of dry sample. Place it in an agate mortar and grind it evenly.
Put it into a mold, press it tightly and scan it. The infrared spectrum of the sample shall
be consistent with the infrared spectrum of the calcium glycerophosphate standard.
Refer to Figure B.1 in Annex B for the infrared spectrum of the calcium
glycerophosphate standard.
A.3 Determination of calcium glycerophosphate content (on a dry basis)
A.3.1 Method summary
In the test solution, calcium carboxylic acid is used as an indicator and titrated with
EDTA-2Na standard titration solution. The content is calculated based on the amount
of EDTA-2Na standard titration solution consumed.
A.3.2 Reagents and materials
A.3.2.1 Sodium chloride.
A.3.2.2 Calcium carboxylate indicator.
A.3.2.3 Sodium hydroxide.
A.3.2.4 Calcium indicator: Weigh 10 g of sodium chloride (A.3.2.1) that has been dried
at 105℃~110℃ for 2 h. Grind it into a fine powder in a mortar. Then add 0.1 g of