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GB 25566-2010 English PDF

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GB 25566-2010: National food safety standards of food additives sodium tripolyphosphate
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GB 25566-2010519 Add to Cart 3 days National food safety standards of food additives sodium tripolyphosphate Obsolete

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Basic data

Standard ID: GB 25566-2010 (GB25566-2010)
Description (Translated English): National food safety standards of food additives sodium tripolyphosphate
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Classification of International Standard: 67.220.20
Word Count Estimation: 13,116
Date of Issue: 2010-12-21
Date of Implementation: 2011-02-21
Regulation (derived from): Ministry of Health Bulletin No. 19 of 2010
Issuing agency(ies): Ministry of Health of the People's Republic of China
Summary: This Chinese standard applies to thermal phosphoric acid and sodium carbonate and sodium tripolyphosphate reaction or recrystallization prepared food additive sodium tripolyphosphate.

GB 25566-2010: National food safety standards of food additives sodium tripolyphosphate

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National food safety standards of food additives sodium tripolyphosphate National Food Safety Standard Food additives Sodium tripolyphosphate Issued on. 2010-12-21 2011-02-21 implementation National Standards of People's Republic of China People's Republic of China Ministry of Health issued

Foreword

Appendix A of this standard is a normative appendix. National Food Safety Standard Food additives Sodium tripolyphosphate

1 Scope

This standard applies to thermal phosphoric acid and sodium carbonate or sodium tripolyphosphate reaction recrystallized prepared food additive sodium tripolyphosphate.

2 Normative references

The standard file referenced in the application of this standard is essential. For dated references, only the dated edition of fitness For this standard. For undated references, the latest edition (including any amendments) applies to this standard.

3 formula and relative molecular mass

Formula 3.1 Na5P3O10 3.2 relative molecular mass 367.86 (according to 2007 international relative atomic mass) 4. Technical Requirements 4.1 Sensory requirements. comply with Table 1. Table 1 Sensory requirements Project requires test methods Color White take appropriate sample is placed in a beaker 50mL watch in natural light Observing the color and texture. Granular or powder state organization 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Sodium tripolyphosphate (Na5P3O10), w /% ≥ 85.0 Appendix A A.4 Total phosphate (as P2O5), w /% 56.0 ~ 58.0 Appendix A A.5 Water-insoluble, w /% ≤ 0.1 A.6 in Appendix A Fluorides (as F)/(mg/kg) ≤ 50 Appendix A A.7 Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.8 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.9 Lead (Pb)/(mg/kg) ≤ 4 Appendix A A.10

Appendix A

(Normative) Testing method A.1 Warning Reagents The standard test methods used for toxic or corrosive, be careful when operating! Such as water splashed on the skin should immediately Flushing, severe cases should be treated immediately. When using volatile acid, to be carried out in a fume hood. When using flammable, do not use open flame heating. A.2 General Provisions This standard reagents and water, did not indicate when the other requirements, refer to three analytical reagent water and GB/T 6682-2008 stipulated. Used in the test standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according to HG/T 3696.2, HG/T Preparation of the provisions of 3696.3. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 hydrochloric acid. A.3.1.2 nitric acid solution. 19. A.3.1.3 ammonia solution. 23. A.3.1.4 silver nitrate solution. 17 g/L. A.3.2 Identification of sodium ions Take a platinum wire, with hydrochloric acid after wetting prior to combustion in the colorless colorless flame. And then dipped in the sample, a colorless combustion flame, the flame that was lit yellow color. A.3.3 phosphate identification method Weigh about 1g sample was dissolved in 20 mL of water, adding a silver nitrate solution to form a yellow precipitate, this precipitate was dissolved in a nitric acid solution or aqueous ammonia solution. A.4 Determination of sodium tripolyphosphate A.4.1 Method summary The sodium tripolyphosphate in a variety of phosphate adsorption on strongly basic anion exchange resin column, using its adsorption on different resins, with no The same concentration of potassium chloride elution to orthophosphate by sequentially pyrophosphates, tripolyphosphates, metaphosphates three outflow, measuring trimerization Sodium content of the eluting solution of phosphorus pentoxide, calculate the content of sodium tripolyphosphate. A.4.2 Reagents and materials A.4.2.1 nitric acid solution. 11. A.4.2.2 hydrochloric acid solution. approximately 2 mol/L. A.4.2.3 buffer solution (pH≈4.3). sodium acetate trihydrate were dissolved 51g (CH3COONa · 3H2O) in water and 46mL glacial acetic acid, diluted with water Diluted to 1000mL. A.4.2.4 ammonium molybdate - sulfuric acid solution. 7.2g/L; Take 7.2 g ammonium molybdate tetrahydrate [(NH4) 6Mo7O24 · 4H2O] was dissolved in water, was added 400mL a concentration of c (1/2H2SO4) = 10 mol/L of Sulfuric acid solution was diluted with water to 1000mL. Sulfuric acid concentration of the solution c (1/2H2SO4) = 4mol/L, per liter containing molybdenum trioxide (MoO3) about 6g. A.4.2.5 ascorbic acid solution. 25g/L, reassortment every 2 to 3 days. A.4.2.6 potassium chloride solution. 0.15mol/L, 0.25mol/L, 0.50mol/L and 0.75mol/L, 1L each concentration solution containing buffer solution (A.4.2.3) 10 mL. A.4.2.7 pentoxide standard solution. 1mL solution containing phosphorous pentoxide (P2O5) 1.00 mg; Take 1.917g (accurate to 0.000 5g) pre-bake at 110 ℃ to 2h potassium dihydrogen phosphate (KH2PO4), dissolved in water and transferred to 1000mL capacity Dilution bottle with water to volume, and mix. A.4.2.8 pentoxide standard solution. 1mL solution containing phosphorous pentoxide (P2O5) 0.01mg; Imbibe 10.00mL pentoxide standard solution (A.4.2.7) in 1000 mL volumetric flask, dilute with water to volume, and mix. A.4.2.9 Quimociac solution. A.4.2.10 ion exchange resins. strong base anion type size or a chlorine-type 0.07mm ~ 0.16mm, and soaked in 4mol/L hydrochloric acid solution to a Zhou water decantation wash lotion to clarify the water stored in the backup. A.4.2.11 glass wool. A.4.3 Instruments and Equipment A.4.3.1 ion exchange column. glass tube inner diameter of 10mm, length 400mm, shrink tube bottom with a glass piston (25mL burette applicable) Figure A.1. Figure A.1 ion exchange column A.4.3.2 separating funnel. 125mL, fixed on the hoop connection with the exchange column at the top. A.4.3.3 sintered glass crucible. filter plate pore size of 5μm ~ 15mμm. A.4.3.4 hard glass test tube. Φ25mm × 200mm. A.4.3.5 water bath, the temperature can be adjusted. A.4.3.6 Spectrophotometer. a wavelength range of 350nm ~ 800nm. A.4.4 Analysis step A.4.4.1 ion exchange column preparation. the ion exchange column is fixed on the shelf, close the piston in the bottom of the column to fill 1cm thick glass wool, pour about 10mL water, resin is injected into a resin bed height of 30cm, with a hydrochloric acid solution immersion spare. The resin used before by the resin regeneration steps of the process It can be injection after treatment. A.4.4.2 resin regeneration. Each sample elution is completed with 200mL of hydrochloric acid solution through the resin bed, the remaining hydrochloric acid solution to be higher than the tree Lipid layer of about 3cm stopped flowing and soak overnight. Then use 50mL hydrochloric acid solution to flow through the column and finally filled, closed-exchange column piston, stuffed with rubber Pusey, overturned several times the resin loose bubble column was discharged vertically fixed on the frame, slow rinse with water resin, and then 5.5mL/min ~ Flow rate 6.0mL/min until the effluent wash has a pH of 4.5 to 5.0 (water approximately 80mL). To maintain the liquid level above the resin layer 1cm, close the oven and dispensing exchange Funnel piston spare. Ion exchange column resin bed is not fizzy; each separation is completed, the resin must be regenerated; and separation in the recycled resin sample the entire process Always keep the column above the liquid resin layer. A.4.4.3 When the resin exchange column or batch parameter changes, adjustment shall select the optimum separation conditions A.4.4.5 program, using samples of known composition, Appropriate choice of elution solution, check the accuracy of column chromatography of ion exchange. A.4.4.4 curve of production. Imbibe pentoxide standard solution (A.4.2.8) 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL, 15.00mL, 20.00mL, 25.00mL, were transferred to a hard glass test tube, diluted with water to 25mL, 10mL added Ammonium molybdate - sulfuric acid solution, 2mL ascorbic acid solution, was heated in a boiling water bath for at least 30min, to ensure complete hydrolysis. Cooling to room temperature, each shift Into 100mL volumetric flask, dilute with water to volume, and mix. With a spectrophotometer at 650nm to 2cm cuvette, measured using water as a reference work The absorbance curve for the series solution. Absorbance absorbance of each solution curve series deductions blank solution as abscissa to pentoxide Phosphorus mass (mg) as ordinate plotted curve. A.4.4.5 choose the best chromatographic conditions. After the selected ion exchange column loaded resin handled well, and then press A.4.4.6 Weigh the sample, Preparation of sample solution, injection, added to the elution solution, each 5mL effluent as a closed, were transferred to a hard glass test tube, diluted with water to 25mL, Add 10mL ammonium molybdate - sulfuric acid solution, 2mL ascorbic acid solution, was heated in a boiling water bath for at least 30min, to ensure complete hydrolysis. Cooling to room temperature Were transferred to 100mL volumetric flask, dilute with water to volume, and mix. With a spectrophotometer at 650nm to 2cm cuvette, using water as a reference, Respectively, the absorbance was measured from the working curve corresponding to Richard pentoxide mass (mg), draw outflow curve to determine the optimal separation strip Member. The selection of the inner diameter of 10mm standard column resin bed height 300mm, column flow rate 5.5mL/min ~ 6.0mL/min, with 0.15mol/L potassium chloride solution 70mL, 0.25mol/L potassium chloride solution 90mL, 0.50mol/L potassium chloride solution 90mL, 75mol/L potassium chloride solution 70mL sequentially eluted positive, coke, Tripolyphosphate, trimetaphosphate phosphate. As shown in Figure A.2. A.4.4.6 preparation of sample solution. Weigh about 1g specimen to the nearest 0.000 2g, dissolved in water and transferred to 500mL volumetric flask, add 10mL Dilution buffer solution with water to volume, and mix (if the turbidity to be filtered). A.4.4.7 Separation Column. Imbibe 10mL sample solution in a separating funnel exchange column end, open exchange column separating funnel and live Plug, so the test solution flows into the resin bed with 10 mL 0.15mol/L potassium chloride solution, rinse the separatory funnel with 60mL 0.15mol/L potassium chloride solution, rinse Resin bed, controlling the flow rate 5.5mL/min ~ 6.0 mL/min, eluent can be discarded; then 90 mL 0.25mol/L potassium chloride solution, rinse the resin bed, Controlling the flow rate 5.5mL/min ~ 6.0 mL/min, eluent can be discarded. With 90mL 0.50mol/L potassium chloride solution elution separation tripolyphosphate component The sodium tripolyphosphate eluate collected in a 400mL beaker high type. A.4.4.8 Determination of phosphorus pentoxide content in the eluate. the eluate tripolyphosphate solution of nitric acid were added 15mL, 70mL water, micro-boiling 40min, Rinse the beaker and watch glass wall, the control test solution volume of about 100mL. And then heated to near boiling, hot add 50mL Quimociac solution, Cover the surface of the dish, boiled for 1min, insulation 30s (in addition of the reagents and the heating process can not use open flame can not be stirred to avoid condensation into Piece). Cooled to room temperature. Use was 180 ℃ ± 5 ℃ drying 45min sand under glass crucible to decantation and filtration, the precipitate was washed three times in a beaker, Water each 15mL, sand and the precipitate transferred to a glass crucible, washed with water to continue (with the wash water of about 150mL). At 180 ℃ ± 5 ℃ dried 45min, or at 250 ℃ ± 5 ℃ dried 15min, cooled to room temperature in a desiccator, and weigh. At the same time a blank test. In addition to the blank test without the sample, the type and amount of addition of reagents and other operating and measured in the same sample. A.4.5 Calculation Results Sodium tripolyphosphate content of sodium tripolyphosphate (Na5P3O10) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated. () () 050 010 55410.0- 01 1 ×× × = mm w (A.1) Where. m1-- sample solution quinoline phosphomolybdate precipitate mass value in grams (g); Numerical quinoline phosphomolybdate precipitation quality m0-- blank test, expressed in grams (g); m - mass of the sample value in units of grams (g); 0.05541-- quinoline phosphomolybdate converted into sodium tripolyphosphate coefficients. Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.5%. Figure A.2 Determination of elution conditions exemplary diagram A.5 Total phosphate (as P2O5) Determination A.5.1 Reagents and materials A.5.1.1 nitric acid solution. 11. A.5.1.2 Quimociac solution. A.5.2 Instruments and Equipment Sintered glass crucible. pore size filtration plate (5 ~ 15) μm. A.5.3 Analysis step Weigh about 1g sample to the nearest 0.000 2g, placed in a beaker l00mL dissolved in water, all transferred to 1000mL volumetric flask with water Dilute to the mark, shake. If necessary, filtration. Pipette 25mL test solution, placed on a high type 400mL beaker, add 15mL nitric acid solution, 70mL Water, micro-boiling 40min, rinse the beaker and watch glass wall, the control test solution volume of about 100mL. And then heated to near boiling, while hot 50mL Quimociac solution, cover the surface of the dish, boiled for 1min, insulation 30s (in addition of the reagents and the heating process can not use fire, Shall not stirred, so as not to clot). Cooled to room temperature. Use was 180 ℃ ± 5 ℃ drying 45min sand under glass crucible filtration decantation, In a beaker precipitate was washed three times with water 15mL, sand and the precipitate transferred to a glass crucible, washed with water to continue (with the wash water of about 150mL), at 180 ℃ ± 5 ℃ dried 45min, or at 250 ℃ ± 5 ℃ dried 15min, cooled to room temperature in a desiccator, and weigh. with When the blank test. In addition to the blank test without the sample, the type and amount of addition of reagents and other operating and measured in the same sample. A.5.4 Calculation Results Total phosphate content of phosphorus pentoxide (P2O5) mass fraction w2 and its value is expressed in%, according to formula (A.2) Calculated. () () 0100025 03,207.001 2 ×× × - = mm w (A.2) Where. m1-- sample solution quinoline phosphomolybdate precipitate mass value in grams (g); Numerical quinoline phosphomolybdate precipitation quality m0-- blank test, expressed in grams (g); m - mass of the sample value in units of grams (g); 0.03207-- quinoline phosphomolybdate converted into phosphorus pentoxide coefficients. Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.3%. A.6 Determination of insoluble matter A.6.1 Instruments and Equipment Sintered glass crucible. filter plate aperture 16μm ~ 40μm. A.6.2 Analysis step Weigh about 10g sample accurate to 0.0lg, placed in 400mL beaker, add 200mL of water, heated to boiling to dissolve, was still hot At 105 ℃ ± 2 ℃ drying to constant quality glass crucible sand filtration, washed with hot water 10 times (each time water about 20mL), washed with phosphate-free to the filtrate Salt (test solution and ammonia nitrates), at 105 ℃ ± 2 ℃ dried to constant mass. A.6.3 Calculation Results Water-insoluble mass fraction w3 and its value is expressed in%, according to formula (A.3) Calculated. 0123 × - = m mmw (A.3) Where. Numerical m1-- sintered glass crucible mass in grams (g); Numerical m2-- water insoluble sand and glass crucible mass in grams (g); m-- sample mass value in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.01%. Determination A.7 fluoride A.7.1 Reagents and materials A.7.1.1 nitric acid solution. 115. A.7.1.2 sodium hydroxide solution. 40 g/L. A.7.1.3 total ionic strength buffer solution (TISAB). using now. A.7.1.4 fluoride standard solution. 1mL solution of fluorine (F) 0.010mg, using now; Pipette Pipette 10mL fluoride standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark, Shake well. With a pipette into the solution of 10mL 100mL flask, diluted with water to the mark. Reserve in a polyethylene bottle. A.7.1.5 bromocresol green indicator solution. A.7.2 Instruments and Equipment A.7.2.1 fluoride ion selective electrode. A.7.2.2 saturated calomel electrode. A.7.2.3 Potentiometers. precision 0.1mV. A.7.2.4 magnetic stirrer. with an outer layer of polyethylene or Teflon stir bar. A.7.3 Analysis step A.7.3.1 Preparation of standard solution of fluorine In five 50mL volumetric flask, with a pipette were added 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL standard fluoride Solution was diluted with water to about 10mL, add 2 drops of bromocresol green indicator solution, adjusted with sodium hydroxide solution or nitric acid solution to the solution just yellow, Added 10mL total ionic strength buffer solution (TISAB), diluted with water to the mark. A.7.3.2 Preparation of test solution Weigh about 1g sample, accurate to 0.01g, was dissolved in 10mL water, 50mL volumetric flask completely shifted, from the following in accordance with A.7.3.1, "added 2 drops bromocresol green indicator solution "to get started. A.7.3.3 Determination The fluoride ion selective electrode and a saturated calomel electrode and a potentiometer connected to the electrode into a beaker filled with water 50mL of polyethylene, preheat Instrument, on a magnetic stirrer with constant stirring, to read the value of the equilibrium potential. Replace the water soak the electrode to electrode potential values specified in the instructions After, it can be the potential standard solution and the sample solution was measured. Equilibrium potential fluoro standard working solution (mV) were measured from low to high concentrations. Fluorine ion concentration (mg/mL) as the value of the abscissa, Corresponding electrode potential value as ordinate, drawing working curve. The same method the equilibrium potential of the sample solution, sample isolated fluorine ion concentration values obtained against the number of fluorine ion concentration from the calibration curve. A.7.4 Calculation Results Fluoride content of fluorine (F) mass fraction w4 and its value in mg/kg according to formula (A.4) Calculated. 3-410 × = cw F (A.4) Where. Fluoride concentrations cF-- value from the working curve according to Richard electrode potential value of the sample solution is measured in milligrams per milliliter (Mg/mL); m - mass of sample values in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 10 mg/kg. A.8 Determination of Arsenic Weigh 1.00g ± 0.01g sample was placed in a conical flask, wetted with water, neutralized with hydrochloric acid to neutral (pH paper test with), and then the excess 5mL, shake. Pipette with a pipette 3mL arsenic standard solution [solution ImL arsenic (As) 1.0μg] as the standard, placed in another conical flask. ......
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