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GB 25565-2010 English PDF

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GB 25565-2010: National food safety standards of food additives trisodium
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GB 25565-2010519 Add to Cart 3 days National food safety standards of food additives trisodium Obsolete

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Basic data

Standard ID: GB 25565-2010 (GB25565-2010)
Description (Translated English): National food safety standards of food additives trisodium
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 industrial thermal phosphoric acid and soda ash or caustic soda reaction of trisodium phosphate food additives.

GB 25565-2010: National food safety standards of food additives trisodium

---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 trisodium National Food Safety Standard Food additives trisodium phosphate 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 Ⅰ II

Foreword

Appendix A of this standard is a normative appendix. National Food Safety Standard Food additives trisodium phosphate

1 Scope

This standard applies to thermal phosphoric acid or caustic soda and soda ash industry prepared by the reaction of trisodium phosphate food additives.

2 Normative references

The 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 mass

Formula 3.1 Anhydrous trisodium phosphate. Na3PO4 Trisodium phosphate monohydrate. Na3PO4 · H2O Trisodium phosphate dodecahydrate. Na3PO4 · 12H2O 3.2 relative molecular mass Anhydrous trisodium phosphate. 163.94 (according to 2007 international relative atomic mass) Trisodium phosphate monohydrate. 181.96 (according to 2007 international relative atomic mass) Trisodium phosphate dodecahydrate. 380.18 (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, observe the color in natural light and Organization status. Crystalline powder or granules state organization 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Anhydrous trisodium phosphate (Na3PO4, to burn dry basis), w /% A trisodium phosphate (Na3PO4 • H2O, to burn dry basis), w /% Dodecahydrate trisodium phosphate (Na3PO4 • 12H2O), w /% 97.0 Appendix A A.4 Table 2. Physical and chemical indicators (cont.) pH (10 g/L solution) 11.5 to 12.5 A.5 in Appendix A Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.6 Fluorides (as F)/(mg/kg) ≤ 50 Appendix A A.7 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.8 Lead (Pb)/(mg/kg) ≤ 4 A.9 in Appendix A Water-insoluble, w /% ≤ 0.2 Appendix A A.10 LOI (Na3PO4), w /% ≤ 2 Appendix A A.11 (Na3PO4 • H2O), w /% 8 ~ 11 (Na3PO4 • 12H2O), w /% 45 ~ 57

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 be treated immediately. A.2 General Provisions The standard test methods and reagents used in water, at the time did not indicate other requirements, refer to analytically pure reagents and GB/T 6682-2008 regulations Given three water. Standard solution, standard solution impurities, formulations and product tests required in the absence of other requirements specified according to HG/T 3696.1, HG/T 3696.2, HG/T 3696.3 regulations of preparation. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 hydrochloric acid. A.3.1.2 acetic acid solution. 11. A.3.1.3 ammonia solution. 23. A.3.1.4 silver nitrate solution. 17 g/L. A.3.2 Analysis step A.3.2.1 Identification of sodium ions Weigh 1g sample, add water to dissolve 20mL. Platinum wire ring dipped in hydrochloric acid, in a colorless flame to burn. And then dipped in a solution of the test flame On combustion, the flame should be bright yellow. A.3.2.2 phosphate ion identification Weigh 0.1 g sample was dissolved in 10 mL of water, add 1 mL silver nitrate solution to produce a yellow precipitate, this precipitate was dissolved in aqueous ammonia solution, not Dissolved in acetic acid solution. A.4 Determination of trisodium phosphate A.4.1 gravimetric method (Arbitration Act) A.4.1.1 Method summary In acidic medium, to Quimociac precipitant solution root test all phosphate Quinoline phosphomolybdate precipitate formed, the precipitate was filtered, Drying, after weighing, trisodium phosphate content in the sample is calculated. A.4.1.2 Reagents and materials A.4.1.2.1 nitrate. A.4.1.2.2 nitrate solution. 1 + 1. A.4.1.2.3 Quimociac solution. A.4.1.3 instruments and equipment A.4.1.3.1 sintered glass crucible. filter plate pore size of 5 μm ~ 15 μm. A.4.1.3.2 electric oven. the temperature can be controlled at 180 ℃ ± 5 ℃ or 250 ℃ ± 10 ℃. A.4.1.4 analysis step A.4.1.4.1 Preparation of test solution It weighs about 2 g anhydrous trisodium phosphate or trisodium phosphate monohydrate sample A.11 ignited (trisodium phosphate dodecahydrate is intact), fine Indeed to 0.000 2 g, placed in 100 mL beaker, dissolved in water all moved into 500 mL volumetric flask, dilute to the mark, shake. A.4.1.4.2 Determination Pipette pipette 15.00 mL test solution was placed in 250 mL beaker, add 10 mL of nitric acid solution, add water to a total volume of about 100 mL, add 50 mL Quimociac solution, cover the surface of the pan, a hot plate or heating in a water bath until the temperature of the cup of 75 ℃ ± 5 ℃, holding 30 s (when not use open flame heating, stirring can not add reagents or heating, so as not to generate a clot). Cooling to room temperature, stirred for 3 cooling process To 4 times. Previously 180 ℃ ± 5 ℃ or 250 ℃ ± 10 ℃ dried to a constant mass of glass sand filtration crucible, first the supernatant was filtered After washing the precipitate by decantation twice with water approximately 20mL, transferred to a sintered glass and the precipitate crucible, crucible and the precipitate was washed with water to continue The inner wall of the crucible several times with the wash water of about 150 mL. Wash was completed, the sand glass crucible placed in the electric oven at 180 ℃ ± 5 ℃ bake 45 min or 250 ℃ ± 10 ℃ bake 15 min, removed, placed in a desiccator to cool to room temperature and weigh to the nearest 0.000 2 g. 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. A.4.1.5 Calculation Results Anhydrous trisodium phosphate or trisodium phosphate monohydrate content of trisodium phosphate (Na3PO4) mass fraction w1 and its value is expressed in% by Equation (A.1) Calculated. () 050015 07408.0) (21 1 ×× × - = mmw (A.1) Trisodium phosphate dodecahydrate content of trisodium phosphate dodecahydrate (Na3PO4 · 12H2O) mass fraction w2 and its value is expressed in% According to formula (A.2) Calculated. () 050015 1718.0) (21 2 ×× × - = mmw (A.2) Where. Numerical quality ml-- test solution was precipitated quinoline phosphomolybdate, in grams (g); Numerical quality m2-- blank test solution was precipitated quinoline phosphomolybdate, in grams (g); m - mass of the sample value in units of grams (g); 0.07408-- quinoline phosphomolybdate converted into a coefficient of anhydrous trisodium phosphate; 0.1718-- quinoline phosphomolybdate terms of trisodium phosphate dodecahydrate coefficient. 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 0.2%. A.4.2 acid-base titration A.4.2.1 Method summary In the sample accurately an excess of hydrochloric acid standard titration solution, titration with standard sodium hydroxide solution to titrate excess hydrochloric acid standard titration solution Fluid, indicating a pH meter jump point, according to the consumption of sodium hydroxide standard titration solution of trisodium phosphate content calculated. A.4.2.2 Reagents and materials A.4.2.2.1 hydrochloric acid standard titration solution. c (HCl) ≈1mol/L. A.4.2.2.2 sodium hydroxide standard titration solution. c (NaOH) ≈1mol/L. A.4.2.3 instruments and equipment A.4.2.3.1 pH meter. Indexing is 0.02; A.4.2.3.2 magnetic stirrer. A.4.2.4 analysis step Weigh about 2.7 g ~ 3.0 g anhydrous trisodium phosphate or trisodium phosphate monohydrate A.11 ignited sample (about 6 trisodium phosphate dodecahydrate g ~ 7 g as is), to the nearest 0.0002 g, into a 400 mL beaker. Dissolved in water plus 40 mL of carbon dioxide-free, with a pipette Accurate added 50.00 mL of hydrochloric acid standard titration solution slowly boiled to remove carbon dioxide, cool. pH meter electrodes into the test has been corrected Test solution, titrated with sodium hydroxide standard solution was titrated to a pH of about 4.0 when the recording sodium hydroxide standard titration solution consumed in the titration Volume V, calculate sample consumption hydrochloric acid standard titrant volume V1. Prevent the solution to absorb carbon dioxide from the air, continue hydroxide Sodium standard solution titration titration solution to a pH of about 8.8, the recording sodium hydroxide standard titration solution consumed by the titration volume V2 (i.e. From pH≈4.0 to pH≈8.8 volume of sodium hydroxide standard titration solution consumed in titration). A.4.2.5 Calculation Results Test solution with hydrochloric acid standard titration solution of hydrochloric acid standard titration solution consumed during titration to pH≈4.0 volume V1, according to the formula (A.3) Calculated. twenty one VccV - = (A.3) Where. After adding 50 mL of hydrochloric acid standard solution titration reaction V-- test solution was titrated with sodium hydroxide standard titration solution to pH≈4.0 when Numerical consumption of sodium hydroxide standard titration solution volume in milliliters (mL); Accurate c1-- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L); Accurate c2-- sodium hydroxide standard titration solution concentration value in units of moles per liter (mol/L). Anhydrous trisodium phosphate or a trisodium phosphate content to burn dry anhydrous trisodium phosphate together (Na3PO4) mass fraction w1 count, the number of Value in%, according to formula (A.4) or formula (A.5) Calculated. When V1c1≥2 V2c2, 0 1 ×× = McVw (A.4) When V1c1 < 2 V2c2 when 0 10) (312,211 1 ×× - = McVcVw (A.5) Trisodium phosphate dodecahydrate content of trisodium phosphate dodecahydrate (Na3PO4 · 12H2O) mass fraction w2 and its value is expressed in% According to the formula (A.6) or formula (A.7) calculated as follows. When V1c1≥2 V2c2, 0 2 ×× = McVw (A.6) When V1c1 < 2 V2c2 when 0 10) (322,211 2 ×× - = McVcVw (A.7) Where. Accurate c1-- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L); Accurate c2-- sodium hydroxide standard titration solution concentration value in units of moles per liter (mol/L); V1-- test solution with hydrochloric acid standard titration solution volume of hydrochloric acid standard titration solution consumed during titration to pH≈4.0 value, single Bit milliliters (mL of); V2-- from pH≈4.0 start with a sodium hydroxide standard titration solution, titration to pH≈8.8 the sodium hydroxide standard titration solution consumed Numerical volume in milliliters (mL); m - mass of the sample value in units of grams (g); M1-- trisodium phosphate (of Na3PO4) molar mass in grams per mole (g/mol) (M1 = 163.94); M2-- twelve trisodium phosphate (Na3PO4 · 12H2O) molar mass in grams per mole (g/mol) (M2 = 380.18). 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 0.2%. A.5 pH measurement A.5.1 Reagents and materials Carbon dioxide-free water. A.5.2 Instruments and Equipment pH meter. Indexing is 0.02. A.5.3 Analysis step Weigh 1.00 g ± 0.01 g sample was placed in 100 mL beaker, with no carbon dioxide dissolved in water and transferred to 100 mL volumetric flask, Dilute to the mark. Poured into 100 mL dry beaker, pH was measured by pH meter test solution. A.6 Determination of Arsenic A.6.1 Reagents and materials A.6.1.1 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.6.1.2 other agents with GB/T 5009.76-2003 Chapter 9. A.6.2 Instruments and Equipment With GB/T 5009.76-2003 Chapter 10. A.6.3 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 The provisions of Chapter 11, "add water to 30 mL" is measured. 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. Determination A.7 fluoride A.7.1 Reagents and materials A.7.1.1 hydrochloric acid solution. 111. A.7.1.2 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.7.1.3 sodium citrate solution. 0.75 mol/L; Weigh 110 g of sodium citrate (Na3C6H5O7 · 2H2O), was dissolved in 300 mL of water, diluted with 14mL of perchloric acid, add water to 500 mL. A.7.1.4 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.7.1.5 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.7.2 Instruments and Equipment With GB/T 5009.18-2003 Chapter 12. A.7.3 Analysis step A.7.3.1 Weigh about 1 g samples, accurate to 0.000 2 g, placed in a 50 mL beaker, add a little water, add 10 mL hydrochloric acid solution, After dissolved and 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.7.3.2 pipette Pipette 1.00 mL, respectively, 2.00 mL, 4.00 mL, 8.00 mL fluoro standard solution, placed in 50 mL volumetric flask, Add 10 mL hydrochloric acid solution and 25 mL of total ionic strength buffer, add water to the mark, shake well and set aside. A.7.3.3 negative terminal fluorine electrode and a saturated calomel electrode and measuring instruments, the positive terminal of the coupling. Electrode into a plastic beaker filled with water, the cup Placed in polyethylene pipe sleeve stirring rod of iron, electromagnetic stirring, the read equilibrium potential value, replace the water 2 to 3 times, the potential value to be balanced After a sample solution can be carried out and the potential of the standard solution was measured. A.7.3.4 ordinate the electrode potential, the quality of fluorine (mg) as the abscissa, drawing working curve on a semi-logarithmic scale, according to a sample Isolated potential value corresponding mass of fluorine on the working curve. A.7.4 Calculation Results Fluoride content of fluorine (F) mass fraction w3 and its value in mg/kg according to formula (A.8) Calculated. 3 10- × = m mw (A.8) 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.8 Determination of Heavy Metals A.8.1 Reagents and materials A.8.1.1 hydrochloric acid solution. 11. A.8.1.2 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.8.1.3 saturated hydrogen sulfide (extemporaneous preparation) water. A.8.1.4 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.8.1.5 phenolphthalein indicator solution. 10 g/L. A.8.2 Instruments and Equipment Colorimetric tube. 50 mL. A.8.3 Analysis step A.8.3.1 Preparation of test solution Weigh 1.00 g ± 0.01 g sample was placed in 50 mL colorimetric tube, add 20 mL of water is dissolved, 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.8.3.2 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.8.3.1, from "Add 5 mL of acetate buffer solution" began simultaneously with the sample treated in the same colorimetric solution. A.9 Determination of Lead A.9.1 Reagents and materials A.9.1.1 4- methyl-2-pentanone (MIBK). A.9.1.2 ammonia solution. 11. A.9.1.3 ammonium sulfate solution. 300 g/L. A.9.1.4 ammonium citrate solution. 250 g/L. A.9.1.5 diethyl dithiocarbamate (DDTC) solution. 50 g/L. A.9.1.6 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.9.1.7 bromothymol blue indicator solution. 1 g/L. A.9.1.8 two Water. comply with GB/T 6682-2008 of. A.9.2 Instruments and Equipment Atomic absorption spectrophotometer. a hollow cathode lamp. A.9.3 Analysis step A.9.3.1 Preparation of test solution Weigh about 5 g samples, accurate to 0.01 g, placed in a 150 mL beaker, all transferred to 125 mL liquid separation after adding 20 mL water to dissolve Funnel, fill with 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 to adjust the pH Solution changed from yellow to blue, add 10 mL of ammonium sulfate solution, 10 mL diethyl dithiocarbamate (DDTC) solution, shake. put Home about 5 min, added 10 mL 4- methyl-2-pentanone (MIBK), shaken vigorously extracted 1 min, after standing layer, the aqueous layer was discarded, 4-methyl-2-pentanone (MIBK) layer into a 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. A.9.3.2 Preparation of standard reference solution than 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.9.3.1 In the steps from the "fill with water to 60 mL" start simultaneously with the sample solution is treated similarly. A.9.3.3 Determination The instrument is adjusted to the best working conditions, water zero. The extract injection, acetylene gas flow can be appropriately reduced, measured at 283.3......
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