GB 1886.356-2022 PDF in English
GB 1886.356-2022 (GB1886.356-2022) PDF English
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National food safety standard - Food additive - Calcium propionate
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Standards related to (historical): GB 1886.356-2022
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GB 1886.356-2022: PDF in English GB 1886.356-2022
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food additive - Calcium
propionate
ISSUED ON: JUNE 30, 2022
IMPLEMENTED ON: DECEMBER 30, 2022
Issued by: National Health Commission;
State Administration for Market Regulation.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Molecular formula, structural formula, relative molecular mass ... 4
3 Technical requirements ... 4
Appendix A Inspection method ... 6
Appendix B Typical chromatogram for the identification of propionic acid ... 14
National food safety standard - Food additive - Calcium
propionate
1 Scope
This standard applies to the food additive - calcium propionate, which is prepared by
neutralization, refining, drying, using propionic acid and calcium hydroxide (or calcium
carbonate or calcium oxide) as raw materials.
2 Molecular formula, structural formula, relative molecular
mass
2.1 Molecular formula
2.2 Structural formula
2.3 Relative molecular mass
186.22 (anhydrous) (according to 2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall meet the requirements of Table 1.
Appendix A
Inspection method
A.1 Warning
Some of the test procedures, which are specified in the test method, may lead to
hazardous situations. Operators shall take appropriate safety and protective measures.
A.2 General provisions
Unless otherwise stated, only reagents confirmed to be analytically pure and grade-3
water, which are specified in GB/T 6682-2008, are used in the analysis. The standard
titration solution, standard solution for impurity determination, preparations and
products, which are used in the test method, shall be prepared in accordance with the
provisions of GB/T 601, GB/T 602, GB/T 603, unless otherwise specified.
A.3 Identification test
A.3.1 Reagents and materials
A.3.1.1 Hydrochloric acid solution: 1 + 3.
A.3.1.2 Sulfuric acid solution: 1 + 9.
A.3.1.3 Oxalic acid solution: 40 g/L.
A.3.1.4 Acetic acid solution: 1 + 20.
A.3.2 Analytical procedures
A.3.2.1 Identification of propionic acid
Weigh 0.5 g of the sample, accurate to 0.01 g. Put it in a 100 mL beaker, which contains
5 mL of water. Stir to dissolve it. Add 5 mL of sulfuric acid solution. When heated,
there shall be a special odor. Determine the main content of calcium propionate,
according to the steps and conditions of A.4. Its typical chromatogram shall conform to
Figure B.1, in Appendix B.
A.3.2.2 Identification of calcium salts
Weigh 0.5 g of sample, accurate to 0.01 g. Put it in a 100 mL beaker, which contains 5
mL of water. Stir to dissolve it. Add oxalic acid solution, then the white precipitate will
be formed. Separate the precipitate. Add acetic acid solution, the precipitate will not
dissolve. Then add hydrochloric acid solution, it can be completely dissolved. Use a
platinum wire which is moistened with hydrochloric acid, to dip the sample, which turns
red in a colorless flame.
A.4 Determination of calcium propionate content (high-performance liquid
chromatography)
A.4.1 Reagents and materials
A.4.1.1 Phosphoric acid.
A.4.1.2 Dihydrogen phosphate.
A.4.1.3 Phosphoric acid solution: 1 mol/L. Add 53.5 mL of phosphoric acid to 50 mL
of water. Mix well. Then add water to, make its volume reach to 1000 mL.
A.4.1.4 Dihydrogen phosphate solution: 1.5 g/L. Weigh 1.5 g of dihydrogen phosphate.
Add water to dissolve and make its volume reach to 1000 mL.
A.4.1.5 Propionic acid standard (C3H6O2): Chromatographically pure, which has a mass
fraction of not less than 99.5%.
A.4.1.6 Standard stock solution of propionic acid: 10 mg/mL. Accurately weigh 1000.0
mg of propionic acid standard, in a 100 mL volumetric flask. Add water to the mark.
Store it in a 4 °C refrigerator, which has a validity period of 6 months.
A.4.2 Instruments and equipment
A.4.2.1 High-performance liquid chromatograph: It is equipped with UV detector or
diode array detector; the sensitivity and stability of the whole machine meet the relevant
provisions in GB/T 16631.
A.4.2.2 Balance: Sensitivity is 0.0001 g and 0.01 g.
A.4.2.3 pH meter.
A.4.3 Analytical procedures
A.4.3.1 Sample preparation and processing
Accurately weigh about 0.2 g (accurate to 0.0001 g) of the sample, which was subject
to drying loss in A.7, into a 500 mL volumetric flask. Add 400 mL of water. Shake well.
Use 1 mol/L phosphoric acid solution, to adjust the pH to about 3.0. Use water to make
its volume reach to the mark. Prepare it into a sample solution.
A.4.3.2 Chromatographic operating conditions
A.4.3.2.1 Chromatographic column: C18 column, 4.6 mm × 250 mm, 5 µm or equivalent
column.
M1 - The molar mass of calcium propionate, in grams per mole (g/mol)
[M(C6H10CaO4) = 186.22];
m - The mass of the weighed specimen, in grams (g);
M2 - The molar mass of propionic acid, in grams per mole (g/mol) [M(C3H6O2) =
74.08];
2 - The conversion factor.
The calculation result retains three significant figures. Take the arithmetic mean of the
two parallel determination results, as the reported result. The absolute difference,
between the two parallel determination results, shall not be greater than 0.5%.
A.5 Determination of water-insoluble content
A.5.1 Instruments and equipment
Glass filter crucible: Filter plate's aperture is 5 µm ~ 15 µm.
A.5.2 Analytical procedures
Weigh 10.0 g of sample, accurate to 0.01 g. Add 100 mL of water. Stir to dissolve it.
Place it for 1 h. Use a glass filter crucible, which has reached constant mass, to filter it.
Use 30 mL of water to wash the filter residue. Dry it at 180 °C ± 2 °C, for 4 h. Weigh it
after cooling.
A.5.3 Result calculation
The mass fraction of water-insoluble matter w2 is calculated, according to formula (A.2).
Where:
m1 - The mass of the filter residue, in grams (g);
m2 - The mass of the weighed sample, in grams (g).
Take the arithmetic mean of the two parallel determination results, as the reported result.
The absolute difference, between the two parallel determination results, is not more
than 0.02%.
A.6 Free acid or free base test
A.6.1 Reagents and materials
A.6.1.1 Sodium hydroxide standard titration solution: c(NaOH) = 0.1 mol/L.
rest half to make it. Fill the vial in the dark. Keep it tightly closed. It is valid for 3
months, after preparation.
A.8.2 Analytical procedures
Weigh 2.0 g of laboratory sample, accurate to 0.01 g. Put it in a 50 mL colorimetric
tube. Add 40 mL of water to dissolve it. Add 2 mL of acetic acid solution. Add water to
50 mL. Add 2 drops of sodium sulfide solution. Place it in a dark place, for 5 min. The
color shall not be darker than the standard colorimetric solution.
Preparation of standard colorimetric solution: Take 2 mL ± 0.02 mL of lead (Pb)
standard solution (0.01 mg/mL). Treat it in the same way as the sample.
A.9 Determination of fluoride
A.9.1 Reagents and materials
A.9.1.1 Perchloric acid.
A.9.1.2 Acetone.
A.9.1.3 Perchloric acid solution: 1 + 100.
A.9.1.4 Sodium hydroxide solution: 40 g/L.
A.9.1.5 Sodium hydroxide solution: 4 g/L.
A.9.1.6 Acetic acid solution: 1 + 16.
A.9.1.7 Silver nitrate solution: 17 g/L.
A.9.1.8 Phenolphthalein indicator solution: 10 g/L.
A.9.1.9 Alizarin ammonia hydroxyl complex solution: Weigh 0.04 g of alizarin
ammonia hydroxyl complex agent. Add a little sodium hydroxide solution (A.9.1.5), to
dissolve it. Use perchloric acid solution, to neutralize it to orange-red (but not forming
emulsion). Use water, to dilute it to 200 mL.
A.9.1.10 Lanthanum perchlorate solution: Weigh 0.04 g of lanthanum oxide. Add 0.25
mL of perchloric acid. Warm to dissolve it. Use water to dilute it to 50 mL.
A.9.1.11 Acetic acid-sodium acetate buffer solution: Weigh 11.0 g of anhydrous sodium
acetate. Add 30 mL of glacial acetic acid and 170 mL of water. Shake until it is dissolved.
A.9.1.12 Compound reagent: Take 60.0 mL of alizarin ammonia hydroxyl complex
solution, 6.0 mL of lanthanum perchlorate solution, 20.0 mL of acetic acid-sodium
acetate buffer solution. Use water, to dilute it to 200 mL.
A.9.1.13 Fluoride (F) standard solution: 0.01 mg/mL.
A.9.2 Analytical procedures
Weigh 5.0 g of sample, accurate to 0.01 g. Put it in a 125 mL distillation flask, which is
equipped with a branch tube. Add a few glass beads. Slowly add 10 mL of perchloric
acid solution, 10 mL of water, 3 ~ 5 drops of silver nitrate solution. The distillation flask
is equipped with a double-hole rubber stopper. Insert a 200 °C thermometer into one
hole; the mercury ball of the thermometer shall be inserted into the test solution. Equip
a separatory funnel to the other hole; a capillary tube is connected underneath; the
capillary tube is inserted into the liquid surface. Connect the branch tube to the
condenser. Connect the outlet of the condenser to a glass elbow. Insert the other end of
the glass elbow into a 100 mL volumetric flask, which contains 10 mL of water, a few
drops of sodium hydroxide (A.9.1.4), 1 drop of phenolphthalein indicator solution;
place the nozzle under the liquid surface. Heat for distillation. Use a separatory funnel,
to add water dropwise to control. Keep the temperature of the test solution, within
135 °C ~ 140 °C. Stop distillation, when the distillate is about 80 mL. Use sodium
hydroxide solution (A.9.1.4), to neutralize the distillate to light red. Then use acetic acid
solution, to neutralize it until colorless. Use water to dilute it to the mark. Shake well.
Take 10 mL into a 50 mL colorimetric tube. Add 5 mL of compound reagent, 6 mL of
acetone. Add water to 50 mL. Shake well. Place it at room temperature for 25 min.
Compare it with the standard colorimetric solution. The blue-purple color shall not be
deeper than the standard colorimetric solution.
Preparation of standard colorimetric solution: Take 1.5 mL ± 0.02 mL of fluoride (F)
standard solution. Treat it at the same time and in the same way as the sample.
A.10 Determination of iron
A.10.1 Reagents and materials
A.10.1.1 Hydrochloric acid.
A.10.1.2 Ammonium persulfate.
A.10.1.3 Ammonium thiocyanate solution: 250 g/L.
A.10.1.4 Iron (Fe) standard solution: 0.01 mg/mL.
A.10.2 Analytical procedure
Weigh 0.5 g of sample, accurate to 0.01 g. Dissolve it in 40 mL of water. Add 2 mL of
hydrochloric acid, 40 mg of ammonium persulfate, 5 mL of ammonium thiocyanate
solution. Shake well. This is the specimen solution.
Preparation of standard colorimetric solution: take 2.5 mL ± 0.02 mL of iron (Fe)
standard solution. Add water to 40 mL. Treat it at the same time and in the same way
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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