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Basic dataStandard ID: GB 25557-2010 (GB25557-2010)Description (Translated English): National food safety standards of food additives sodium pyrophosphate Sector / Industry: National Standard Classification of Chinese Standard: X42 Classification of International Standard: 67.220.20 Word Count Estimation: 12,160 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 (soda ash) or caustic sodium hydroxide (burn shout) and the reaction of the food additive sodium pyrophosphate. GB 25557-2010: National food safety standards of food additives sodium pyrophosphate---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.National food safety standards of food additives sodium pyrophosphate National Food Safety Standard Food additive sodium pyrophosphate 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 ForewordAppendix A of this standard is a normative appendix. National Food Safety Standard Food additive sodium pyrophosphate1 ScopeThis standard applies to industrial thermal phosphoric acid and sodium carbonate (soda ash) or caustic sodium hydroxide (caustic soda) and obtained by the reaction of food additives Agent is sodium pyrophosphate.2 Normative reference standardThe standard file referenced in the application of this standard is essential. For dated references, only the edition date of the note Apply to this standard. For undated references, the latest edition (including any amendments) applies to this standard.3 formula and relative molecular massFormula 3.1 Anhydrous sodium pyrophosphate. Na4P2O7 Sodium pyrophosphate decahydrate. Na4P2O7 · 10H2O 3.2 relative molecular mass Anhydrous sodium pyrophosphate. 265.90 (according to 2007 international relative atomic mass) Sodium pyrophosphate decahydrate .. 446.10 (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 50mL beaker was observed under natural light Color and texture. Powder or crystalline state organization 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Sodium pyrophosphate decahydrate (Na4P2O7 • 10H2O), w /% ≥ 98.0 Appendix A A.4 Anhydrous sodium pyrophosphate (Na4P2O7), w /% 96.5 ~ 100.5 Orthophosphate by test A.5 in Appendix A pH (10 g/L solution) 9.9 ~ 10.7 A.6 in Appendix A Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.7 Table 2. Physical and chemical indicators (cont.) Item Index Test Method Fluorides (as F)/(mg/kg) ≤ 50 Appendix A A.8 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.9 Lead (Pb)/(mg/kg) ≤ 4 Appendix A A.10 Water-insoluble, w /% ≤ 0.2 Appendix A A.11 Burning Reductions (Na4P2O7 • 10H2O), w /% 38.0 ~ 42.0 Appendix A A.12 (Na4P2O7) a, w /% ≤ 0.5 a. loss on ignition (Na4P2O7) index of factory test indicators.Appendix A(Normative) Testing method A.1 Warning Reagents The standard test methods used for toxic or corrosive, be careful when operating! If necessary, to be in the hood Carried out. As splashed on the skin should immediately wash with water, severe cases should seek medical care immediately. A.2 General Provisions The standard test methods used in the reagents and water in the absence of other specified requirements, refer to analytically pure reagents and GB/T 6682-2008 Three water regulations. Used in the test standard titration solution, impurity standard solution, preparations and products, did not indicate when additional requirements are Press HG/T 3696.1, HG/T 3696.2, the provisions of HG/T 3696.3 of preparation. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 hydrochloric acid. A.3.1.2 nitric acid solution. 11. A.3.1.3 acetic acid solution. 11. A.3.1.4 ammonia solution. 23. A.3.1.5 silver nitrate solution. 17 g/L. A.3.2 Analysis step A.3.2.1 Identification of sodium ions Weigh 1 g sample add 20 mL of water to dissolve, with platinum wire ring dipped in hydrochloric acid after wetting, the flame to colorless. Test solution and then dipped in fire The flame burning, the flame should be bright yellow. A.3.2.2 pyrophosphate ion discrimination Sample solution A.3.2.2.1. 0.1g sample was dissolved in 100mL the nitric acid solution; A.3.2.2.2 Test solution A. in 30mL Quimociac added dropwise 0.5mL sample solution; A.3.2.2.3 Test solution B. The remaining sample solution was heated at 95 ℃ 10min, take 0.5mL of this solution was added dropwise a solution of 30mL Quimociac in; A.3.2.2.4 determination. Test solution B immediately formed yellow precipitate A test solution does not appear. A.4 Determination of sodium pyrophosphate A.4.1 Method summary Sodium pyrophosphate with hydrochloric acid disodium dihydrogen pyrophosphate, zinc sulfate was added to the solution, and the precipitate was quantitatively generated zinc pyrophosphate acid, Standard titration with sodium hydroxide solution to titrate the resulting sulfuric acid, and then calculated based on the consumption of sodium pyrophosphate containing sodium hydroxide standard titration solution the amount. A.4.2 Reagents and materials A.4.2.1 hydrochloric acid solution. 20 + 1. A.4.2.2 zinc sulfate solution. 125 g/L; The 125 g of zinc sulfate (ZnSO4 · 7H2O) were dissolved in water and diluted with water to 1 L, the pH meter, depending on the pH of the display, with sulfur Acid solution (1 + 500) or sodium hydroxide solution (6 g/L) was adjusted to pH 3.8. A.4.2.3 anhydrous sodium pyrophosphate; a) of anhydrous sodium pyrophosphate as an industrial method for preparing the starting material. The first crystallization. Weigh 30 g of anhydrous sodium pyrophosphate industry, placed in 400 mL beaker, add 100 mL of water, heated to dissolve, with the Speed quantitative filter paper. The filtrate was cooled in a cold water bath, crystalline precipitation, the solution was decanted, washed with a small amount of water and crystallized twice. Second crystallization. the first crystallization with a small amount of water dissolved by heating in a cold water bath cooling, precipitated crystals were decanted solution. Third Crystallization. the second crystallization second crystallization method by recrystallization once. b) sodium pyrophosphate decahydrate reagent method of preparing the starting material. Weigh 80 g of sodium pyrophosphate decahydrate reagent, according to a) of the first and second crystallization operations. The above recrystallization sodium pyrophosphate into a porcelain crucible, at 400 ℃ for burning to a constant quality. A.4.2.4 sodium hydroxide standard titration solution. c (NaOH) = 0.1 mol/L. Calibration. Weigh about 0.5 g of anhydrous sodium pyrophosphate (A.4.2.3), accurate to 0.000 2 g, placed in 250 mL beaker, add 90 mL of water Was dissolved, the solution was added hydrochloric acid solution was adjusted to pH 3.8 with stirring. Added 50 mL zinc sulfate solution, stirred 5 min, stirring with hydrogen Sodium hydroxide standard titration solution titrated to a solution of pH 3.6 to stop near the titration, the solution was stirred for 2 min to reach equilibrium, continue titration to pH 3.8, then add a drop of each to mix after 30 s. 0.1 mol per ml/L sodium hydroxide standard titration solution of sodium pyrophosphate equivalent mass (ρ) in grams per milliliter (g/mL) said, according to Equation (A.1) Calculated. m = ρ (A.1) Where. m1-- weighed anhydrous sodium pyrophosphate quality value in units of grams (g); Numerical V1-- sodium hydroxide standard titration solution consumed in the calibration volume in milliliters (mL). A.4.3 Instruments and Equipment A.4.3.1 titrator or a pH meter. Indexing is 0.01 mV or 0.02. A.4.3.2 magnetic stirrer. A.4.4 Analysis step Weigh about 5 g samples, accurate to 0.000 2 g, the sample is dissolved in water, transferred to a 500 mL volumetric flask, dilute to the mark and shaken, If necessary, filtration. With pipette 50 mL of the test solution was placed in 250 mL beaker, add 40 mL of water, stirring slowly added a solution of hydrochloric Solution pH 3.8, and then press the step in A.4.2.4, from "zinc sulfate solution was added 50 mL" Start calibration. A.4.5 Calculation Results Anhydrous sodium pyrophosphate content of sodium pyrophosphate (Na4P2O7) mass fraction w1 and its value is expressed in%, according to formula (A.2) Calculated. () 05005021 ×× = m Vw ρ (A.2) Decahydrate sodium pyrophosphate content of sodium pyrophosphate decahydrate (Na4P2O7 · 10H2O) mass fraction w2 and its value is expressed in%, according to public Formula (A.3) Calculated. () 050 050 678.12 1 ×× × = Vw ρ (A.3) Where. ρ-- per milliliter of sodium hydroxide standard titration solution of anhydrous sodium pyrophosphate equivalent mass in grams per milliliter (g/mL); Numerical sodium hydroxide standard titration solution consumed V2-- titration solution volume in milliliters (mL); Numerical m-- sample mass, expressed in grams (g); 1.678-- anhydrous sodium pyrophosphate, sodium pyrophosphate decahydrate in terms of 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%. Note. This method is only used for the determination of sodium pyrophosphate, polyphosphates when there exists, this method is not accurate. A.5 orthophosphate test A.5.1 Reagents and materials Silver nitrate solution. 17 g/L. A.5.2 Analysis step Weigh 1.0 g of sample into powder, add 2 drops to 3 drops of silver nitrate solution may not be noticeable yellow. A.6 pH measurement of A.6.1 Reagents and materials Carbon dioxide-free water. A.6.2 Instruments and Equipment pH meter. Indexing is 0.02. A.6.3 Analysis step The reference electrode and the measuring electrode and pH meter connected, preheating, zero, location. Weigh 1.00 g ± 0.01 g sample was placed in 100 mL Beaker, no carbon dioxide dissolved in water, all moved into 100 mL volumetric flask, dilute to the mark. Pour 100 mL dry Beaker, pH was measured by pH test solution. A.7 Determination of Arsenic A.7.1 Reagents and materials A.7.1.1 arsenic standard solution. 1 mL solution of arsenic (As) 0.001 mg; Pipette 1.00 mL of arsenic standard solution according to HG/T 3696.2 requirements formulated and placed in 1000 mL volumetric flask, dilute with water to the mark, Shake well. The solution is using now. A.7.1.2 other agents with GB/T 5009.76-2003 Chapter 9. A.7.2 Instruments and Equipment With GB/T 5009.76-2003 Chapter 10. A.7.3 Analysis step Weigh 1.00 g ± 0.01 g sample was placed in measuring arsenic flask, add 6 mL of hydrochloric acid was dissolved, following in GB/T 5009.76-2003 first From the provisions of Chapter 11, "add water to 30 mL" from the measurement. Mercuric bromide paper Gutzeit was the color can not be deeper than the standard. Limits formulated solution. Pipette 3.00 mL of arsenic standard solution, and treated in the same sample at the same time. A.8 Determination of fluoride A.8.1 Reagents and materials A.8.1.1 hydrochloric acid solution. 111. A.8.1.2 sodium acetate solution. 3 mol/L; Weigh 204 g of sodium acetate (CH3COONa · 3H2O), was dissolved in 300 mL of water, add 1 mol/L acetic acid solution to adjust the pH to 7.0, Diluted with water to 500 mL. A.8.1.3 sodium citrate solution. 0.75 mol/L; Weigh 110 g of sodium citrate (Na3C6H5O7 · 2H2O), was dissolved in 300 mL of water, add 14 mL of perchloric acid, and then diluted with water to 500 mL. A.8.1.4 total ionic strength buffers. Sodium acetate solution (3 mol/L) and sodium citrate solution (0.75 mol/L) were mixed equally, temporary use when the current formulation. A.8.1.5 fluoride standard solution. 1 mL solution of fluorine (F) 0.010 mg. Pipette 1.00 mL of fluoride standard solution according to HG/T 3696.2 requirements formulated and placed in 100 mL volumetric flask, dilute to the mark with water Degree, shake. A.8.2 Instruments and Equipment With GB/T 5009.18-2003 Chapter 12. A.8.3 Analysis step A.8.3.1 Weigh about 1 g samples, accurate to 0.0002 g, placed in a 50 mL beaker, add a little water, add 10 mL of hydrochloric acid solution, boil 1 min, after rapid cooling, it was transferred to a 50 mL volumetric flask, add 25 mL of total ionic strength buffer, add water to the mark, shake well and set aside. A.8.3.2 Pipette 1.00 mL, respectively, 2.00 mL, 5.00 mL, 10.00 mL of fluoride standard solution, placed in 50 mL volumetric flask, add 10 mL solution of hydrochloric acid and 25 mL of total ionic strength buffer, add water to the mark, shake well and set aside. A.8.3.3 fluorine electrode and the negative terminal calomel electrode and measuring instruments, the positive terminal of the coupling. Electrode into a plastic beaker filled with water, and put the cup With a magnetic stir bar on a magnetic stirrer with constant stirring, to read the value of the equilibrium potential, the replacement of 2 to 3 times after water until it reaches the electrode description After a predetermined potential value of the book can be a sample solution and standard solution was measured potential. A.8.3.4 equilibrium potential fluoro standard working solution from low to high concentrations were measured. Ordinate the electrode potential, the quality of fluorine (mg) Abscissa, drawing working curve on a semi-logarithmic scale. The same method the equilibrium potential of the test solution, the concentration of fluoride ions in the sample (mg/mL), isolated from the working curve. A.8.4 Calculation Results Fluoride content of fluorine (F) mass fraction w3 and its value in mg/kg according to formula (A.4) Calculated. 3 10- × = m mw (A.4) Where. Numerical quality test solution m1-- isolated from the working curve of fluorine in milligrams (mg); 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 5 mg/kg. A.9 Determination of Heavy Metals A.9.1 Reagents and materials A.9.1.1 hydrochloric acid solution. 11. A.9.1.2 acetate buffer solution. pH≈3.5; Weigh 25.0 g ammonium acetate, add 25 mL dissolved, add 45 mL hydrochloric acid solution, then dilute hydrochloric acid or dilute ammonia water to adjust the pH to 3.5 with Diluted with water to 100 mL. A.9.1.3 saturated hydrogen sulphide water (use namely distribution). A.9.1.4 Lead standard solution. 1 mL solution containing lead (Pb) 0.010 mg; Pipette 1.00 mL of lead standard solution according to HG/T 3696.2 prepared, placed in 100 mL volumetric flask, dilute to the mark, shake. The solution was prepared prior to use. A.9.1.5 phenolphthalein indicator solution. 10 g/L. A.9.2 Instruments and Equipment Colorimetric tube. 50 mL. A.9.3 Analysis step A.9.3.1 Preparation of test solution Weigh 1.00 g ± 0.01 g sample was placed in 50 mL colorimetric tube, add 20 mL of water to dissolve. Add 1 drop of phenolphthalein indicator solution, acid-soluble salt Solution and to the solution is colorless, add 5 mL of acetate buffer solution, 10 mL of saturated hydrogen sulphide water, diluted with water to the mark. In the dark Placed at 10 min, color can not be deeper than the standard colorimetric solution was. A.9.3.2 Preparation of standard colorimetric solution Pipette 1.00 mL of lead standard solution, placed in 50 mL colorimetric tube, add 20 mL of water, then press the steps described in A.9.3.1, from "Add 5 mL of acetate buffer solution" Start with the test solution at the same time the same treatment. A.10 Determination of Lead A.10.1 reagents and materials A.10.1.1 4- methyl-2-pentanone (MIBK). A.10.1.2 ammonia solution. 11. A.10.1.3 ammonium sulfate solution. 300 g/L; Weigh 30 g of ammonium sulfate, dissolved in water and add water to 100 mL. A.10.1.4 ammonium citrate solution. 250 g/L; Weigh 25 g of ammonium citrate, dissolved in water and add water to 100 mL. A.10.1.5 diethyl dithiocarbamate (DDTC) solution. 50 g/L; Weigh 5 g diethyl dithiocarbamate, dissolved in water and add water to 100 mL. A.10.1.6 lead standard solution. 1 mL solution containing lead (Pb) 0.010 mg; Pipette 1.00 mL of lead standard solution according to HG/T 3696.2 requirements formulated and placed in 100 mL volumetric flask, dilute with water to the mark, Shake well. A.10.1.7 bromothymol blue indicator solution. 1 g/L. A.10.1.8 two Water. comply with GB/T 6682-2008 of. A.10.2 instruments and equipment Atomic absorption spectrophotometer. a lead hollow cathode lamp. A.10.3 Analysis steps A.10.3.1 prepared test solution Weigh about 5 g samples, accurate to 0.01 g, placed in a 150 mL beaker, add 20 mL of water after the transfer was dissolved to 125 mL separating funnel The additional water to 60 mL, add 2 mL of ammonium citrate solution, 3 drops to 5 drops of bromothymol blue indicator solution with aqueous ammonia solution was adjusted to pH solution Change from yellow to blue, add 10 mL of ammonium sulfate solution, 10 mL diethyl dithiocarbamate (DDTC) solution, shake. Place 5 min About adding 10.0 mL 4- methyl-2-pentanone (MIBK), shaken vigorously extracted 1 min, after standing layer, the aqueous layer was discarded, the MIBK Layer into 10 mL stoppered graduated tube, and set aside. Meanwhile blank test, in addition to the blank test solution without the sample, the other kind and amount of addition of the reagents with the same test solution. Preparation of standard solutions A.10.3.2 Pipette respectively lead standard solution 0.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, placed in 125 mL separating funnel, then press A.10.3.1 In the steps from the "fill with water to 60 mL" start simultaneously with the test solution the same treatment. A.10.4 Determination The instrument is adjusted to the best working conditions, water zero. The extract injection, acetylene gas flow can be appropriately reduced in at 283.3 nm Measured absorbance of standard solution, test solution and the blank test solution. Subtracting the absorbance of zero standard solution from the absorbance of each standard solution, the quality of lead (mg) as abscissa and the corresponding absorbance The vertical axis, drawing working curve. According to the test solution and the absorbance measured blank test solution, check the quality of lead from the working curve. A.10.5 Calculation Results Lead content of lead (Pb) mass fraction w4 and its value in mg/kg according to formula (A.5) Calculated. 4 10- × - = mm w (A.5) Where. Numerical test solution quality lead m1-- isolated from the working curve, in milligrams (mg); Numerical blank test solution m0-- isolated from the working curve lead mass in milligrams (mg); 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 1 mg/kg. A.11 Determination of insoluble matter A.11.1 instruments and equipment A.11.1.1 sintered glass crucible. filter plate pore size of 5 μm ~ 15 μm. A.11.1.2 electric oven. control temperature 105 ℃ ± 2 ℃. A.11.2 Analysis steps Weigh approximately 20 g samples, accurate to 0.01 g, placed in 400 mL beaker, add 200 mL of water and dissolved by heating at 105 ℃ with advance ± 2 ℃ under constant quality glass crucible sand filtration, washed with hot water until the filtrate was no alkaline. The sand glass crucible placed in 105 ℃ ± 2 ℃ Power Hot thermostatic oven dried to constant mass. A.11.3 Calculation Results Water-insoluble mass fraction w5 and its value is expressed in%, according to formula (A.6) Calculated. 0015 × - = m mm w (A.6) Where. Numerical m1-- water insoluble sand and glass crucible mass in grams (g); Numerical m0-- sintered glass crucible mass in grams (g); m-- sample mass value in grams (g). 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