GB 1886.45-2016 English PDF

GB 1886.45-2016: Food additive -- Calcium chloride
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GB 1886.45-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Additives - Calcium
Chloride
ISSUED ON: AUGUST 31, 2016
IMPLEMENTED ON: JANUARY 1, 2017
Issued by: National Health and Family Planning Commission of the People’s
Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Molecular Formula and Relative Molecular Mass ... 4
3 Technical Requirements ... 4
Appendix A Inspection Method ... 6
National Food Safety Standard - Food Additives - Calcium
Chloride
1 Scope
This Standard is applicable to food additive calcium chloride.
2 Molecular Formula and Relative Molecular Mass
2.1 Molecular Formula
Anhydrous calcium chloride: CaCl2
Calcium chloride dihydrate: CaCl2  2H2O
2.2 Relative Molecular Mass
Anhydrous calcium chloride: 110.98 (in accordance with the international relative atomic mass
of 2007)
Calcium chloride dihydrate: 147.01 (in accordance with the international relative atomic mass
of 2007)
3 Technical Requirements
3.1 Sensory Requirements
The sensory requirements shall comply with the requirements of Table 1.
3.2 Physical and Chemical indicators
The physical and chemical indicators shall comply with the provisions of Table 2.
Appendix A
Inspection Method
A.1 Safety Tips
Some of the reagents used in this test method are toxic or corrosive and shall be handled with
caution. If they splash on the skin, immediately use water to rinse them. If the situation is serious,
immediately seek medical treatment.
A.2 General Provisions
Unless otherwise specified, the reagents and water used in this Standard refer to analytically
pure reagents and Grade-3 water specified in GB/T 6682. The standard solutions, impurity
standard solutions, preparations and products required in the tests, unless otherwise specified,
shall be prepared in accordance with the provisions of GB/T 601, GB/T 602 and GB/T 603. The
solutions used in the tests refer to aqueous solutions, unless the solvent used is specified.
A.3 Identification Test
A.3.1 Reagents and materials
A.3.1.1 Hydrochloric acid solution: 1 + 11.
A.3.1.2 Ammonium oxalate solution: 35 g/L.
A.3.1.3 Ammonia water: 1 + 3.
A.3.1.4 Silver nitrate solution: 10 g/L.
A.3.1.5 Methyl red indicator solution: 1 g/L.
A.3.2 Identification method for calcium salts
Take about 0.2 g of specimen and add 10 mL of water to dissolve it. This solution is used as
specimen solution A (for identification of calcium salts and chlorides).
Take an appropriate amount of specimen solution A, add 2 drops of methyl red indicator
solution, use ammonia water to neutralize it, and add ammonium oxalate solution to generate a
white precipitate. This precipitate dissolves in hydrochloric acid, but not in acetic acid.
A.3.3 Identification method for chlorides
Take specimen solution A and add silver nitrate solution to generate a white precipitate, which
is insoluble in nitric acid.
A.4 Determination of Calcium Chloride
V---the volume of the ethylenediaminetetraacetic acid disodium salt standard titration solution
consumed by titrating the test solution, expressed in (mL);
V0---the volume of the ethylenediaminetetraacetic acid disodium salt standard titration solution
consumed in the blank test, expressed in (mL);
M---the molar mass of calcium chloride, expressed in (g/mol), [M (CaCl2) = 111.0; M (CaCl2 
2H2O) = 147.0];
m---the mass of the specimen, expressed in (g);
10---the volume of the test solution taken and transferred, expressed in (mL);
500---the total volume of the test solution, expressed in (mL);
1,000---conversion factor.
The arithmetic mean of the parallel determination results shall prevail in the test result. The
absolute difference between two independent determination results obtained under repeatability
conditions is not greater than 0.2%.
A.5 Determination of Free Alkali [Ca(OH)2]
A.5.1 Method summary
Dissolve the specimen in water, add excess hydrochloric acid standard titration solution and
boil to drive out carbon dioxide. Use bromothymol blue as an indicator and use sodium
hydroxide standard titration solution to titrate the excess hydrochloric acid.
A.5.2 Reagents and materials
A.5.2.1 Hydrochloric acid standard titration solution: c (HCl) = 0.1 mol/L.
A.5.2.2 Sodium hydroxide standard titration solution: c (NaOH) = 0.1 mol/L.
A.5.2.3 Bromothymol blue indicator solution: 1 g/L.
A.5.3 Analytical steps
Weigh-take about 10 g of specimen, accurate to 0.01 g, place in a 400 mL beaker, and add an
appropriate amount of water to dissolve it. Add 2 ~ 3 drops of bromothymol blue indicator and
use a burette to add hydrochloric acid standard titration solution to neutralize it, with an excess
of about 5 mL. Accurately record the volume of the hydrochloric acid standard titration solution.
Heat and boil it for 2 minutes, then, add 2 drops of bromothymol blue indicator solution and
use sodium hydroxide standard titration solution to titrate it, until the color turns from yellow
to blue, which is the end point.
A.5.4 Result calculation
The mass fraction w2 of free alkali [Ca(OH)2] is calculated in accordance with Formula (A.2):
Where,
c1---the concentration of hydrochloric acid standard titration solution, expressed in (mol/L);
V1---the volume of hydrochloric acid standard titration solution added during titration,
expressed in (mL);
c2---the concentration of sodium hydroxide standard titration solution, expressed in (mol/L)
V2---the volume of sodium hydroxide standard titration solution consumed during titration,
expressed in (mL);
M1---the molar mass of calcium hydroxide, expressed in (g/mol), {M [ଵଶ CaሺOHሻଶ] = 37.05}
m1---the mass of the specimen, expressed in (g).
The arithmetic mean of the parallel determination results shall prevail in the test result. The
absolute difference between two independent determination results obtained under repeatability
conditions is not greater than 0.05%.
A.6 Determination of Magnesium and Alkali Metal Salts
A.6.1 Method summary
The specimen solution is added with oxalic acid in an ammonia solution to generate a calcium
oxalate precipitate and separate the calcium. Evaporate the solution to dryness and burn it. The
residue is magnesium and alkali metal salts.
A.6.2 Reagents and materials
A.6.2.1 Ammonium chloride.
A.6.2.2 Oxalic acid solution: 63 g/L.
A.6.2.3 Ammonia solution: 1 + 3.
A.6.2.4 Methyl red indicator solution: 1 g/L.
A.6.3 Analytical steps
Weigh-take about 1 g of specimen, accurate to 0.01 g, place it in a 250mL beaker and add 50
mL of water to dissolve it. Add 500 mg of ammonium chloride, then, boil for 1 min. Quickly
add 40 mL of oxalic acid solution and vigorously stir it to generate a precipitate. Immediately
to room temperature, dissolve it in water, transfer it into a 100 mL volumetric flask. Use water
to dilute it to the scale, shake it well, and store it in a refrigerator for later use.
A.7.2.5 Fluorine standard working solution: 1 mL of solution contains 10 g of fluorine (F).
Transfer-take 1 mL of fluorine standard solution into a 100 mL volumetric flask, use water to
dilute it to the scale, and shake it well. The solution shall be prepared just before use.
A.7.3 Instruments and equipment
A.7.3.1 Fluorine electrode.
A.7.3.2 Acidity meter.
A.7.3.3 Magnetic stirrer.
A.7.3.4 Calomel electrode.
A.7.4 Analytical steps
Preparation of standard solution: transfer-take 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL, 5.0 mL and 6.0
mL of fluorine standard working solution respectively into six 50 mL volumetric flasks,
respectively add 5 mL of hydrochloric acid solution, 10 mL of sodium citrate solution and 10
mL of ethylenediaminetetraacetic acid disodium salt solution, add water to the scale, and shake
them well.
Preparation of specimen solution: weigh-take 1.00 g  0.01 g of specimen, place in a 250 mL
beaker, add water to dissolve it, transfer all to a 100 mL volumetric flask, use water to dilute to
the scale, and shake it well. Transfer-take 10 mL of the specimen solution into a 50 mL
volumetric flask, add 5 mL of hydrochloric acid solution, 10 mL of sodium citrate solution and
10 mL of ethylenediaminetetraacetic acid disodium salt solution, add water to the scale and
shake it well.
Connect the calomel electrode and the fluorine electrode to the measurement instrument, insert
the electrodes into a 25 mL plastic beaker filled with water, under electromagnetic stirring, read
the potential value, replace the water 2 ~ 3 times, and after the potential value is balanced,
successively measure the potential value of the standard solution from low concentration to
high concentration, and the potential value of the specimen solution.
With the electrode potential as the ordinate and the mass (μg) of fluorine in 50 mL of solution
as the abscissa, draw a working curve on semi-logarithmic coordinate paper. In accordance with
the potential value of the specimen solution, the mass of fluorine in the specimen solution is
obtained from the working curve.
A.7.5 Result calculation
The mass fraction w4 of fluorine (F) is calculated in accordance with Formula (A.4):
GB 1886.45-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Additives - Calcium
Chloride
ISSUED ON: AUGUST 31, 2016
IMPLEMENTED ON: JANUARY 1, 2017
Issued by: National Health and Family Planning Commission of the People’s
Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Molecular Formula and Relative Molecular Mass ... 4
3 Technical Requirements ... 4
Appendix A Inspection Method ... 6
National Food Safety Standard - Food Additives - Calcium
Chloride
1 Scope
This Standard is applicable to food additive calcium chloride.
2 Molecular Formula and Relative Molecular Mass
2.1 Molecular Formula
Anhydrous calcium chloride: CaCl2
Calcium chloride dihydrate: CaCl2  2H2O
2.2 Relative Molecular Mass
Anhydrous calcium chloride: 110.98 (in accordance with the international relative atomic mass
of 2007)
Calcium chloride dihydrate: 147.01 (in accordance with the international relative atomic mass
of 2007)
3 Technical Requirements
3.1 Sensory Requirements
The sensory requirements shall comply with the requirements of Table 1.
3.2 Physical and Chemical indicators
The physical and chemical indicators shall comply with the provisions of Table 2.
Appendix A
Inspection Method
A.1 Safety Tips
Some of the reagents used in this test method are toxic or corrosive and shall be handled with
caution. If they splash on the skin, immediately use water to rinse them. If the situation is serious,
immediately seek medical treatment.
A.2 General Provisions
Unless otherwise specified, the reagents and water used in this Standard refer to analytically
pure reagents and Grade-3 water specified in GB/T 6682. The standard solutions, impurity
standard solutions, preparations and products required in the tests, unless otherwise specified,
shall be prepared in accordance with the provisions of GB/T 601, GB/T 602 and GB/T 603. The
solutions used in the tests refer to aqueous solutions, unless the solvent used is specified.
A.3 Identification Test
A.3.1 Reagents and materials
A.3.1.1 Hydrochloric acid solution: 1 + 11.
A.3.1.2 Ammonium oxalate solution: 35 g/L.
A.3.1.3 Ammonia water: 1 + 3.
A.3.1.4 Silver nitrate solution: 10 g/L.
A.3.1.5 Methyl red indicator solution: 1 g/L.
A.3.2 Identification method for calcium salts
Take about 0.2 g of specimen and add 10 mL of water to dissolve it. This solution is used as
specimen solution A (for identification of calcium salts and chlorides).
Take an appropriate amount of specimen solution A, add 2 drops of methyl red indicator
solution, use ammonia water to neutralize it, and add ammonium oxalate solution to generate a
white precipitate. This precipitate dissolves in hydrochloric acid, but not in acetic acid.
A.3.3 Identification method for chlorides
Take specimen solution A and add silver nitrate solution to generate a white precipitate, which
is insoluble in nitric acid.
A.4 Determination of Calcium Chloride
V---the volume of the ethylenediaminetetraacetic acid disodium salt standard titration solution
consumed by titrating the test solution, expressed in (mL);
V0---the volume of the ethylenediaminetetraacetic acid disodium salt standard titration solution
consumed in the blank test, expressed in (mL);
M---the molar mass of calcium chloride, expressed in (g/mol), [M (CaCl2) = 111.0; M (CaCl2 
2H2O) = 147.0];
m---the mass of the specimen, expressed in (g);
10---the volume of the test solution taken and transferred, expressed in (mL);
500---the total volume of the test solution, expressed in (mL);
1,000---conversion factor.
The arithmetic mean of the parallel determination results shall prevail in the test result. The
absolute difference between two independent determination results obtained under repeatability
conditions is not greater than 0.2%.
A.5 Determination of Free Alkali [Ca(OH)2]
A.5.1 Method summary
Dissolve the specimen in water, add excess hydrochloric acid standard titration solution and
boil to drive out carbon dioxide. Use bromothymol blue as an indicator and use sodium
hydroxide standard titration solution to titrate the excess hydrochloric acid.
A.5.2 Reagents and materials
A.5.2.1 Hydrochloric acid standard titration solution: c (HCl) = 0.1 mol/L.
A.5.2.2 Sodium hydroxide standard titration solution: c (NaOH) = 0.1 mol/L.
A.5.2.3 Bromothymol blue indicator solution: 1 g/L.
A.5.3 Analytical steps
Weigh-take about 10 g of specimen, accurate to 0.01 g, place in a 400 mL beaker, and add an
appropriate amount of water to dissolve it. Add 2 ~ 3 drops of bromothymol blue indicator and
use a burette to add hydrochloric acid standard titration solution to neutralize it, with an excess
of about 5 mL. Accurately record the volume of the hydrochloric acid standard titration solution.
Heat and boil...