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GB 1886.335-2021: National food safety standard - Food additives - Sodium tripolyphosphate
GB 1886.335-2021
National food safety standard-Food additives-Sodium tripolyphosphate
National Standards of People's Republic of China
National Food Safety Standard
Food additive sodium tripolyphosphate
Released on 2021-02-22
2021-08-22 implementation
National Health Commission of the People's Republic of China
Issued by the State Administration for Market Regulation
National Food Safety Standard
Food additive sodium tripolyphosphate
1 Scope
The standard is applicable to the food additive trimer produced with sodium carbonate (or sodium hydroxide) and food additive phosphoric acid (including wet-process phosphoric acid) as raw materials
Sodium phosphate, or sodium tripolyphosphate, a food additive produced by recrystallization from sodium tripolyphosphate.
2 Molecular formula and relative molecular mass
2.1 Molecular formula
Na5P3O10
2.2 Relative molecular mass
367.86 (according to.2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements should meet the requirements of Table 1.
Table 1 Sensory requirements
3.2 Physical and chemical indicators
The physical and chemical indicators should meet the requirements of Table 2.
Appendix A
Testing method
Warning. Some reagents used in this standard test method are toxic or corrosive.
Rinse immediately with water, and treat severe cases immediately. For reagents that contain highly toxic drugs, they should be managed strictly in accordance with relevant regulations, and avoid inhalation when using them.
Into or contact with the skin, if necessary, it should be carried out in a fume hood, and people with wounds in the exposed parts should not touch it. When using volatile acids,
Proceed in a fume hood. When using flammable products, it is strictly forbidden to use an open flame for heating.
A.1 General provisions
The reagents and water used in this standard refer to analytical reagents and tertiary water specified in GB/T 6682 when no other requirements are indicated. test
The standard solutions, preparations and products used in the test for impurity determination shall be in accordance with GB/T 601, GB/T 602, and GB/T 601, unless other requirements are specified.
Prepared according to GB/T 603.The solution used refers to an aqueous solution when it is not specified which solvent is used for preparation.
A.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Hydrochloric acid.
A.2.1.2 Nitric acid solution. 18.
A.2.1.3 Ammonia solution. 1 1.
A.2.1.4 Sodium hydroxide solution. 40g/L.
A.2.1.5 Silver nitrate solution. 17g/L.
A.2.2 Identification method
A.2.2.1 Identification of sodium ions
Take the platinum wire, moisten it with hydrochloric acid, and burn it on a colorless flame until it is colorless, then dip the sample and burn it in a colorless flame, and the flame will appear bright
yellow.
A.2.2.2 Identification of phosphate
Weigh about 0.2g of the sample, dissolve it in 20mL of water, take 1mL on the watch glass, add a few drops of silver nitrate solution, and a yellow precipitate should be formed.
This precipitate is soluble in ammonia solution or nitric acid solution.
A.3 Determination of sodium tripolyphosphate (Na5P3O10) content
A.3.1 Method summary
The various phosphates in sodium tripolyphosphate are adsorbed on the strong basic anion exchange resin column, and the adsorption capacity is different.
The potassium chloride solution is eluted to make it flow out in the order of ortho, coke, trimer, trimetaphosphate, and determine the phosphorus pentoxide in the sodium tripolyphosphate eluate
Calculate the content of sodium tripolyphosphate.
A.3.2 Reagents and materials
A.3.2.1 Nitric acid solution. 11.
A.3.2.2 Hydrochloric acid solution. about 2mol/L.
A.3.2.3 Buffer solution (pH≈4.3). Dissolve 51g of sodium acetate trihydrate (CH3COONa·3H2O) and 46mL of glacial acetic acid in water
In, dilute with water to 1000mL.
A.3.2.4 Ammonium molybdate-sulfuric acid solution. 7.2g/L. Dissolve 7.2g ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in water and add
400mL sulfuric acid solution with concentration c(1/2H2SO4)=10mol/L, dilute with water to 1000mL. The concentration of sulfuric acid in this solution is
c(1/2H2SO4)=4mol/L, each liter contains about 6g molybdenum trioxide (MoO3).
A.3.2.5 Ascorbic acid solution. 25g/L, reconstituted every 2d~3d.
A.3.2.6 Potassium chloride solution. 0.15mol/L, 0.25mol/L, 0.50mol/L and 0.75mol/L, each concentration solution contains buffer solution in 1L
Solution (A.3.2.3) 10mL.
A.3.2.7 Phosphorus pentoxide standard stock solution. 1mL solution contains 1.00mg of phosphorus pentoxide (P2O5). Put potassium dihydrogen phosphate (KH2PO4) in
Bake at 110℃±2℃ for 2h. After cooling in a desiccator, weigh out 1.917g (accurate to 0.0005g), add water to dissolve, transfer to 1000mL capacity
In the bottle, dilute to the mark with water and mix well.
A.3.2.8 Phosphorus pentoxide standard solution. 1mL solution contains 0.01mg of phosphorus pentoxide (P2O5). Accurately draw 10.0mL of two pentoxide
Phosphorus standard solution (A.3.2.7) in a 1000mL volumetric flask, dilute to the mark with water, and mix.
A.3.2.9 Quinomolimonone solution. Weigh 70g of sodium molybdate and dissolve it in 150mL of water to form solution 1.Weigh 60g of citric acid and dissolve it in
In a mixture of 150mL water and 85mL nitric acid, it is solution 2.While stirring, slowly add solution 1 to solution 2, which is solution 3.in
Add 5mL quinoline to the mixture of 35mL nitric acid and 100mL water, which is solution 4.Add solution 4 to solution 3, stir evenly, and put
Leave for 24h, filter, add 280mL acetone to the filtrate, dilute to 1000mL with water, and mix.
Warning. This solution should be stored in a polyethylene bottle. This solution contains acetone and should not be used near the flame. If heating or boiling during operation
Should be carried out in a fume hood.
A.3.2.10 Ion exchange resin. strong alkaline anion type, chlorine type, particle size 0.07mm~0.16mm, immersed in 4mol/L hydrochloric acid solution
Soak for one week, wash with water by decantation until the lotion is clear, and store it in the aqueous solution for later use.
A.3.2.11 Glass wool.
A.3.3 Instruments and equipment
A.3.3.1 Ion exchange column. The glass tube has an inner diameter of 10mm, a length of 400mm, and the bottom of the tube shrinks. It is equipped with a glass piston, as shown in Figure A.1.
A.3.3.2 Separation funnel. 125mL, fixed on the iron ring and connected to the top of the exchange column.
A.3.3.3 Glass sand crucible. The pore size of the filter plate is 5μm~15μm.
A.3.3.4 Hard glass test tube. ϕ25mm×200mm.
A.3.3.5 Water bath. controllable to slightly boiling.
A.3.3.6 Electric heating constant temperature drying oven. The temperature control range is 180℃±2℃ or 250℃±5℃.
A.3.3.7 Spectrophotometer. The wavelength range is 350nm~800nm.
A.3.4 Analysis steps
A.3.4.1 Preparation of ion exchange column
Fix the ion exchange column on the shelf, close the piston, fill the bottom of the column with 1cm thick glass wool, and pour about 10mL of water to soak it.
Pour the resin into the column so that the height of the resin bed is 30cm, and immerse it with hydrochloric acid solution for later use. The resin is treated according to the resin regeneration step before use
After the process is processed, the sample can be injected.
The volume of the test solution is controlled to be approximately 100 mL. Then heat to near boiling, add 50mL quinmolimonone solution while it is hot, cover with a watch glass, and heat
Boiling for 1min, keep for 30s (during the process of adding reagents and heating, do not use open flame, do not stir, so as not to condense into lumps). Cool down to the room
temperature. Use a glass sand crucible that has been dried at 180°C±2°C for 45 minutes to filter by decantation, and wash the precipitate 3 times in a beaker, each time
Water 15mL, transfer the precipitate into the glass sand crucible, and continue to wash with water (the washing water used is about 150mL). Put the glass sand crucible together with the sink
The deposit is placed in an electric heating constant temperature drying box, starting from the temperature stabilization, and drying at 180℃±2℃ for 45min, or at 250℃±5℃
Dry for 15min, cool in a desiccator, and weigh. At the same time, a blank test is carried out.
Except for the blank test without adding the sample, the other operations and the type and amount of reagents added are the same as those for the test sample.
A.3.5 Result calculation
The mass fraction w1 of sodium tripolyphosphate (Na5P3O10) is calculated according to formula (A.1).
w1=
(m1-m0)×0.05541×500
m2×10
×100% (A.1)
Where.
m1 ---The mass of the quinoline phosphomolybdate precipitate of the sample solution, in grams (g);
m0 ---The mass of the quinoline phosphomolybdate precipitate in the blank test, in grams (g);
0.05541 ---The coefficient of conversion of quinoline phosphomolybdate to sodium tripolyphosphate;
500 --- the volume of the volumetric flask, in milliliters (mL);
m2 --- the mass of the sample, in grams (g);
10 --- Pipette the volume of the sample solution, in milliliter (mL).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 0.5%.
A.4 Determination of total phosphate (as P2O5)
A.4.1 Reagents and materials
A.4.1.1 Nitric acid solution.1 1.
A.4.1.2 Quinomolimidone solution.
A.4.2 Instruments and equipment
A.4.2.1 Glass sand crucible. The aperture of the filter plate is 5μm~15μm.
A.4.2.2 Electric heating constant temperature drying oven. The temperature control range is 180℃±2℃ or 250℃±5℃.
A.4.3 Analysis steps
Weigh about 1g sample, accurate to 0.0002g, put it in a 100mL beaker, add water to dissolve, and transfer all to a 1000mL volumetric flask.
Dilute to the mark with water and shake well. Filter if necessary. Pipette 25mL test solution, put it in a 400mL tall beaker, add 15mL nitric acid
Solution and 70mL water, boil slightly for 40min, rinse the watch glass and the wall of the beaker with water, and control the volume of the test solution to be about 100mL. Reheat to
Near boiling, add 50mL quinmolybdenone solution while it is hot, cover with a watch glass, heat and boil for 1 min, keep it for 30s (after adding reagents and heating
During the process, do not use open flame, do not stir, so as not to condense into lumps). Cool to room temperature. Use those that have been dried at 180℃±5℃ for 45min
The glass sand crucible is suction filtered by decantation method, and the precipitate is washed 3 times in a beaker with 15 mL of water each time, and the precipitate is moved into the glass sand crucible, and continue to use
Wash with water (approximately 150 mL of washing water used). Put the glass sand crucible together with the precipitate in the electric heating constant temperature drying box, and start counting from the stable temperature.
When drying at 180℃±5℃ for 45min, or at 250℃±5℃ for 15min, cool in a desiccator and weigh. Simultaneously
Blank test.
Except for the blank test without adding the sample, the other operations and the type and amount of reagents added are the same as those for the test sample.
A.4.4 Result calculation
The mass fraction w2 of total phosphate (calculated as P2O5) is calculated according to formula (A.2).
w2=
(m3-m4)×0.03207×1000
m5×25
×100% (A.2)
Where.
m3 ---The mass of the quinoline phosphomolybdate precipitate of the sample solution, in grams (g);
m4 ---The mass of the quinoline phosphomolybdate precipitate in the blank test, in grams (g);
0.03207 ---The coefficient of conversion of quinoline phosphomolybdate to phosphorus pentoxide;
1000 --- the volume of the volumetric flask, in milliliters (mL);
m5 --- the mass of the sample, in grams (g);
25 --- Pipette the volume of the sample solution, the unit is milliliters (mL).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 0.3%.
A.5 Determination of water insoluble matter
A.5.1 Instruments and equipment
A.5.1.1 Glass sand crucible. The aperture of the filter plate is 16μm~40μm.
A.5.1.2 Electric heating constant temperature drying oven. The temperature control range is 105℃±2℃.
A.5.2 Analysis steps
Weigh about 10g of the sample, accurate to 0.01g, place it in a 400mL beaker, add.200mL of water, heat it to boiling to dissolve it, and use it while it is hot
Dried to a glass sand crucible with constant quality at 105℃±2℃, and filtered with suction, washed with hot water 10 times (about 20mL of water each time), and washed the sink
Precipitate to the filtrate without phosphate (test with silver nitrate solution and ammonia solution), and place it in an electric thermostatic drying oven at 105℃±2℃ to dry to
Constant quality.
A.5.3 Result calculation
The mass fraction w3 of water-insoluble matter is calculated according to formula (A.3).
w3=
m6-m7
m8
×100% (A.3)
Where.
m6---The mass of water insoluble matter and glass sand crucible, in grams (g);
m7---the mass of the glass sand crucible, in grams (g);
m8---The mass of the sample, in grams (g).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 0.01%.
A.6 Determination of pH (10g/L aqueous solution)
A.6.1 Reagents and materials
Carbon dioxide-free water.
A.6.2 Apparatus and equipment
Acidity meter. resolution of 0.01pH, equipped with glass electrode and saturated calomel electrode (or composite electrode).
A.6.3 Analysis steps
Weigh 1.00g±0.01g sample, place it in a 100mL beaker, dissolve it with carbon dioxide-free water, and transfer it into a 100mL volumetric flask.
Dilute to the mark with carbon dioxide-free water and shake well. Pour into a 100mL dry beaker, measure the sample solution with a calibrated acidity meter
的pH.