GB 1886.332-2021 English PDF (GB1886.332-2021)

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GB 1886.332-2021: National food safety standard - Food additives - Calcium phosphate tribasic
GB 1886.332-2021
National food safety standard-Food additives-Calcium phosphate tribasic
National Standards of People's Republic of China
National Food Safety Standard
Food additive tricalcium phosphate
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
Preface
This standard replaces GB 25558-2010 "National Food Safety Standard Food Additive Tricalcium Phosphate".
Compared with GB 25558-2010, the main changes of this standard are as follows.
---Modified the scope;
--- Amend "fluoride (in F)" to "fluorine (F)";
---Modify the fluorine inspection method to GB/T 5009.18;
--- Modify the lead inspection method to the first method of GB 5009.75-2014 or the second method, third method, and third method of GB 5009.12-2017
Four methods;
---Modify the inspection method of arsenic to GB 5009.76 or GB 5009.11;
---Revised the inspection method of heavy metals to GB 5009.74.
National Food Safety Standard
Food additive tricalcium phosphate
1 Scope
This standard applies to the food additive phosphorus produced with calcium hydroxide (or calcium carbonate) and food additive phosphoric acid (including wet-process phosphoric acid) as raw materials.
Tricalcium phosphate is also suitable for the food additive tricalcium phosphate produced with calcium chloride solution and trisodium phosphate as raw materials.
2 Molecular formula and relative molecular mass
2.1 Molecular formula
Approximate composition. 10CaO·3P2O5·H2O
2.2 Relative molecular mass
1004.61 (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.
Table 2 Physical and chemical indicators
Appendix A
Testing method
Warning. Some reagents used in this test method are toxic or corrosive.
In progress. If it splashes on the skin, it should be rinsed with water immediately, and the severe cases should be treated immediately.
A.1 General provisions
The reagents and water used in this standard refer to analytical reagents and the tertiary water specified in GB/T 6682 when other requirements are not specified.
The standard titration solution, standard solution for impurity determination, preparations and products used in the test, unless other requirements are specified, are in accordance with GB/T 601,
Preparation according to GB/T 602 and 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 Nitric acid solution. 11.
A.2.1.2 Hydrochloric acid solution. 13.
A.2.1.3 Ammonia solution. 1 1.
A.2.1.4 Ammonium oxalate solution. 35g/L.
A.2.1.5 Ammonium molybdate solution. 60g/L, weigh 6g of ammonium molybdate [(NH4)6MO7O24·4H2O] and dissolve in 50mL of water, while stirring
Slowly add 50mL nitric acid solution and store in a brown reagent bottle.
A.2.2 Identification method
A.2.2.1 Identification of calcium ions
Weigh about 0.1g sample, add 5mL hydrochloric acid solution, 5mL water, heat to 40℃~50℃, add 1mL ammonia water while stirring
Solution, add 5mL ammonium oxalate solution, produce white precipitate.
A.2.2.2 Identification of phosphate
Weigh about 0.1g sample, add nitric acid solution dropwise to dissolve the sample, then excess 1mL nitric acid solution, heat to 40℃~50℃, add
10mL of ammonium molybdate solution produced a yellow precipitate.
A.3 Determination of the content of tricalcium phosphate (calculated as Ca)
A.3.1 Direct titration method with disodium ethylenediaminetetraacetic acid (EDTA) (Method 1)
A.3.1.1 Method summary
Dissolve the sample with hydrochloric acid solution, add triethanolamine solution as a masking agent to mask the influence of interfering ions, and add ethyl acetate dropwise under acidic conditions.
The standard titration solution of disodium diaminetetraacetic acid (EDTA) is near the end point, and the pH of the sample solution is adjusted to the hydroxynaphthol blue index with sodium hydroxide solution.
In the pH range of the indicator color, continue to titrate the remaining calcium.
A.3.1.2 Reagents and materials
A.3.1.2.1 Triethanolamine.
A.3.1.2.2 Hydrochloric acid solution. 11.
A.3.1.2.3 Sodium hydroxide solution. 450g/L.
A.3.1.2.4 Disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution. c(EDTA)=0.05mol/L.
A.3.1.2.5 Hydroxynaphthol blue indicator. Weigh 10g of sodium chloride dried at 105℃±2℃ for 2h, put it in a mortar, add 0.1g
Hydroxynaphthol blue indicator, grind and mix well. Place it in a weighing bottle and store in a desiccator. The use period is 2 months.
A.3.1.3 Instruments and equipment
Magnetic stirrer.
A.3.1.4 Analysis steps
Weigh 0.15g sample, accurate to 0.0002g, and place it in a 250mL beaker equipped with a magnetic stirrer, and add a small amount of water to moisten the sample.
Wet, add 5mL hydrochloric acid solution to dissolve it, if necessary, slowly heat it, carefully add 125mL water, and add 0.5mL three
Ethanolamine and 0.3g hydroxynaphthol blue indicator, use a burette to add EDTA standard titration solution dropwise at a normal speed
23mL~27mL (the amount added should be equivalent to 90%~95% of the calcium content), dropwise add sodium hydroxide solution until the initial red turns blue, and then
Continue to drip until the blue turns purple, and then an excess of 0.5mL, at this time the pH of the solution should be between 12.3~12.5.Continue to use ethylenediaminetetraacetic acid
Disodium (EDTA) standard titration solution was titrated until the solution appeared clear blue and kept unchanged for 60 seconds. 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 (except the standard titration solution) are the same as the determination test.
A.3.1.5 Result calculation
The mass fraction w1 of tricalcium phosphate (calculated as Ca) is calculated according to formula (A.1).
w1=
[(V1-V0)/1000]×c1×M1
m1
×100% (A.1)
Where.
V1 --- The volume of EDTA standard titration solution consumed by the titration of the sample solution, in milliliters
(mL);
V0 --- The volume of EDTA standard titration solution consumed in the blank test, in milliliters (mL);
1000---conversion factor;
c1 ---The concentration of ethylenediaminetetraacetic acid disodium (EDTA) standard titration solution, the unit is moles per liter (mol/L);
M1 --- The molar mass of calcium (Ca) in grams per mole (g/mol) [M1=40.078];
m1 --- 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 0.2%.
A.3.2 Zinc sulfate back titration method (Method 2)
A.3.2.1 Method summary
In the sample solution, add an excess of the standard titration solution of disodium ethylenediaminetetraacetic acid to complex with calcium ions, and use the KB mixture as an indicator
Reagent, use zinc sulfate standard titration solution to titrate excess disodium ethylenediaminetetraacetic acid standard titration solution.
A.3.2.2 Reagents and materials
A.3.2.2.1 Hydrochloric acid solution. 11.
A.3.2.2.2 Ammonia-ammonium chloride buffer solution (A). pH≈10.
A.3.2.2.3 Disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution. c(EDTA)=0.05mol/L.
A.3.2.2.4 Acid chrome blue K-naphthol green B mixed indicator liquid (KB indicator liquid).
A.3.2.2.5 Zinc sulfate standard titration solution. c(ZnSO4·7H2O)=0.05mol/L.
Preparation. Weigh 15g of zinc sulfate, add water to dissolve, dilute to 1000mL with water, and shake well.
Calibration. Pipette 25.00mL prepared zinc sulfate standard titration solution, put it in an Erlenmeyer flask, add 10mL ammonia-ammonium chloride buffer solution
(A) And 75mL water, add about 0.02g chrome black T indicator, use 0.05mol/L disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution
Titrate until the solution turns from purple to pure blue, and keep the color unchanged for 30s, which is the end point. 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 (except the standard titration solution) are the same as the determination test.
The concentration of zinc sulfate standard titration solution c2, the unit is moles per liter (mol/L), calculated according to formula (A.2).
c2=
(V2-V3)×c3
V4
(A.2)
Where.
V2---The volume of the standard titration solution of disodium ethylenediaminetetraacetic acid (EDTA) consumed in the titration, in milliliters (mL);
V3---The volume of the standard titration solution of disodium ethylenediaminetetraacetic acid (EDTA) consumed in the blank test, in milliliters (mL);
c3---The concentration of disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution, the unit is moles per liter (mol/L);
V4--Pipette the volume of the standard titration solution of zinc sulfate, the unit is milliliters (mL).
A.3.2.3 Analysis steps
Weigh about 0.5g sample, accurate to 0.0002g, place it in a 100mL beaker, moisten it with a small amount of water, and add 5mL hydrochloric acid solution to make the test
All the samples are dissolved. Transfer all to a 250mL volumetric flask, dilute to the mark with water, and shake well. Dry filter if necessary, discard the first 20mL
filtrate.
Pipette 25.00mL of the above sample solution, place it in a 500mL Erlenmeyer flask, and use another pipette to transfer 25.00mL ethylenediaminetetraethyl
Disodium acid (EDTA) standard titration solution, add 50mL water, 10mL ammonia-ammonium chloride buffer solution (A), shake well, and place for 5min. Add 2 drops
~3 drops of KB indicator solution, titrated with zinc sulfate standard titration solution until the solution changes from blue to blue-purple, and keeps it for 30s without fading, that is the end
point. 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 (except the standard titration solution) are the same as the determination test.
A.3.2.4 Result calculation
The mass fraction w1 of tricalcium phosphate (calculated as Ca) is calculated according to formula (A.3).
w1=
[(V5-V6)/1000]×c4×M2
m2×25/250
×100% (A.3)
Where.
V5 --- The volume of the zinc sulfate standard titration solution consumed in the blank test, in milliliters (mL);
V6 --- The volume of the zinc sulfate standard titration solution consumed by the titration of the sample solution, in milliliter (mL);
1000---conversion factor;
c4 --- The concentration of zinc sulfate standard titration solution, in moles per liter (mol/L);
M2 --- The molar mass of calcium (Ca) in grams per mole (g/mol) [M2=40.078];
m2 --- the mass of the sample, in grams (g);
25 --- Pipette the volume of the sample solution, the unit is milliliters (mL);
250 --- The volume of the sample solution at a constant volume, in 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 0.2%.
A.4 Determination of ignition loss
A.4.1 Instruments and equipment
A.4.1.1 Porcelain crucible. 30mL.
A.4.1.2 High temperature furnace. The temperature control range is 800℃±50℃.
A.4.2 Analysis steps
Use a porcelain crucible that has been burned at 800 ℃ ± 50 ℃ for 30 minutes, weigh about 2g sample, accurate to 0.0002g, and place it in a high-temperature furnace.
Burn at 800℃±50℃ for 30min, take it out, cool to room temperature, and weigh.
A.4.3 Result calculation
The mass fraction w2 of ignition loss is calculated according to formula (A.4).
w2=
m3-m4
m5
×100% (A.4)
Where.
m3---The mass of the sample and crucible before ignition, in grams (g);
m4---The mass of residue and crucible after ignition, in grams (g);
m5---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 0.1%.
A.5 Determination of clarity
A.5.1 Reagents and materials
A.5.1.1 Hydrochloric acid solution.1 1.
A.5.1.2 Nitric acid solution. 12.
A.5.1.3 Silver nitrate solution. 20g/L.
A.5.1.4 Chloride standard solution. 1mL solution contains 0.010mg of chlorine (Cl). Pipette 10.00mL of chlorine prepared according to GB/T 602
Compound standard solution, placed in a 100mL volumetric flask, dilute to the mark with water, and shake well. The solution is ready to use.
A.5.2 Apparatus and equipment
Constant temperature water bath.
A.5.3 Analysis steps
Preparation of standard turbidity solution. Pipette 6.0mL chloride standard solution, place it in a 50mL colorimetric tube, add 20mL water, 1mL nitrate
Acid solution, 1mL silver nitrate solution, dilute to the mark with water, shake well. Place it in a dark place for 15 minutes.
Weigh 2.00g±0.01g sample, place it in a 50mL beaker, add 18mL water and 8mL hydrochloric acid solution, and heat it in a boiling water bath
Dissolve in 5min. After cooling, transfer all to a 50mL colorimetric tube, dilute to the mark with water, and shake well. The turbidity of the sample solution is not greater than the standard
A quasi-turbid solution is a pass test.
A.6 Determination of lead (Pb)
Measure according to the method specified in the first method of GB 5009.75-2014 or the second method, third method and fourth method of GB 5009.12-2017,
The water used in the test is the secondary water specified in GB/T 6682.
A.7 Determination of Arsenic (As)
Measure according to the method specified in GB 5009.76 or GB 5009.11, a...