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GB 25563-2010 English PDF

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GB 25563-2010: Tripotassium phosphate of the national food safety standards of food additives
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GB 25563-2010519 Add to Cart 3 days Tripotassium phosphate of the national food safety standards of food additives Obsolete

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Basic data

Standard ID: GB 25563-2010 (GB25563-2010)
Description (Translated English): Tripotassium phosphate of the national food safety standards of food additives
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Classification of International Standard: 67.220.20
Word Count Estimation: 13,155
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 potassium hydroxide or potassium carbonate reaction of the food additive potassium phosphate.

GB 25563-2010: Tripotassium phosphate of the national food safety standards of food additives

---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.
Tripotassium phosphate of the national food safety standards of food additives National Food Safety Standard Food additives tripotassium 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

Foreword

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

1 Scope

This standard applies to thermal phosphoric acid and potassium hydroxide or potassium carbonate prepared food additive tripotassium phosphate.

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 tripotassium phosphate. K3PO4 Hydrated tripotassium phosphate. K3PO4 · nH2O 3.2 relative molecular mass Anhydrous tripotassium phosphate. 212.27 (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 Tripotassium phosphate (K3PO4) (burning dry basis), w /% ≥ 97.0 Appendix A A.4 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) ≤ 10 Appendix A A.7 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.8 Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.9 Table 2. Physical and chemical indicators (cont.) Item Index Test Method Water-insoluble, w /% ≤ 0.2 Appendix A A.10 LOI Anhydrous, w /% ≤ 5.0 Appendix A A.11 Hydrate, w /% 8.0 ~ 20.0

Appendix A

(Normative) Testing method A.1 Warning Reagents used in this test method are toxic or corrosive, be careful when operating! If necessary, to be carried out in a fume hood. As splashed on the skin should immediately wash with water, severe cases should be treated immediately. A.2 General Provisions This standard reagents and water, did not indicate when the other requirements, refer to the three water analytical reagent and GB/T 6682-2008 requirements. Test the required standard solution, impurity standard solution, preparations and products, in the absence of other requirements specified according to HG/T 3696.1, HG/T 3696.2 requiring 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 ethanol. 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.3.1.6 solution of sodium hydrogen tartrate. 110. A.3.2 Analysis step A.3.2.1 Identification of potassium 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 Flame on the burner, in cobalt glass, the flame should be purple. In neutral, the appropriate concentration or concentrated solution of potassium salt, sodium hydrogen tartrate solution was added slowly to give a white precipitate, this precipitate was dissolved Aqueous ammonia solution and an alkaline solution, adding a small amount of acetic acid or ethanol will accelerate the generation of precipitation. A.3.2.2 Identification of phosphate 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 tripotassium 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, the sample is calculated tripotassium phosphate content. 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 sand glass crucible. filter plate pore size 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 Weigh about 2 g sample after A.11 by burning, to the nearest 0.000 2 g, placed in 100 mL beaker, all moved into 250 mL dissolved in water Volumetric flask, dilute to the mark, shake. A.4.1.4.2 Determination Pipette pipette 10.00 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 (Not use an open flame when heated, add the reagent can not be stirred or heated, so as not to generate a clot). Cooling to room temperature, the cooling process was stirred for 3 to 4 Times. Previously 180 ℃ ± 5 ℃ or 250 ℃ ± 10 ℃ dried to a constant mass of glass sand filtration crucible, the supernatant was filtered finish first, with The precipitate was washed by decantation twice, each time with water of about 20 mL, the precipitate was transferred to a sintered glass crucible, the precipitate was washed with water and continue to the inner wall of the crucible Many times, the use of wash water of about 150 mL. Wash was completed, the sand glass crucible placed in electric oven, and bake at 180 ℃ ± 5 ℃ 45 min Or 250 ℃ ± 10 ℃ bake 15 min, removed, cooled to room temperature and placed in a desiccator 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 Tripotassium phosphate, tripotassium phosphate (K3PO4) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated. () 025 010 09592.0) (21 1 ×× × - = mmw (A.1) 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 - the value of the sample mass, in grams (g); Quinoline phosphomolybdate 0.09592-- tripotassium converted into a 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 calculated tripotassium phosphate content. A.4.2.2 Reagents and materials A.4.2.2.1 hydrochloric acid standard titration solution. c (HCl) = 1 mol/L. A.4.2.2.2 sodium hydroxide standard titration solution. c (NaOH) = 1 mol/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 4 g sample after A.11 by burning, to the nearest 0.000 2 g, placed in 400 mL beaker, add 40 mL of carbon dioxide-free Water solubility. Pipette accurately added 50.00 mL of hydrochloric acid standard titration solution slowly boiled to remove carbon dioxide, cool. The corrected The pH meter electrode in the test solution, titrated with sodium hydroxide standard solution was titrated to a pH of about 4.0, the recording titration consumption hydroxide Sodium standard titration solution volume V, calculate sample consumption hydrochloric acid standard titrant volume V1. Prevent the solution absorb carbon from the air CFCs continue titrated with sodium hydroxide standard titration solution to a pH of about 8.8, the recording standard sodium hydroxide consumed in the titration Titration solution volume V2 (from sodium hydroxide standard titration pH≈4.0 to pH≈8.8 titration solution consumed volume). A.4.2.5 Calculation Results Test solution was titrated with hydrochloric acid standard solution titration to pH≈4.0 when hydrochloric acid standard titration solution consumed volume V1, according to the formula (A.2) Calculated. twenty one VccV - = (A.2) 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). Tripotassium phosphate content of tripotassium phosphate (K3PO4) mass fraction w1 and its value is expressed in%, according to formula (A.3) or formula (A.4) Calculated. When V1c1≥2 V2c2, 0 1 ×× = McVw (A.3) When V1c1 < 2 V2c2 when 0 10) (32211 1 ×× - = McVcVw (A.4) 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 - the value of the sample mass, in grams (g); M-- tripotassium phosphate (K3PO4) molar mass in grams per mole (g/mol) (M = 212.27). 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 100mL beaker, with no carbon dioxide dissolved in water and transferred to 100 mL volumetric flask, Diluted with water 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 3 of Chapter 9 5009.76-200. 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 bottle, add dissolved 6mL hydrochloric acid, following in GB/T 5009.76-2003 first The provisions of Chapter 11, "add water to 30mL" were determined. 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, add 14 mL of perchloric acid, and then diluted with 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 3 g samples, accurate to 0.000 2 g, placed in a 50 mL beaker, add a little water, add 10 mL hydrochloric acid solution, dissolved After the solution transferred to a 50 mL volumetric flask, sealed soak extraction 1 h (gentle shaking from time to time), should be avoided on the sample stick the bottle wall. mention After adding 25 mL of total ionic strength buffer, add water to the mark, shake well and set aside. A.7.3.2 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 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 in the cup Polyethylene pipe sleeve placed iron stir bar after electromagnetic stirring, the reading equilibrium potential value, replace 2 to 3 times the water, the potential value to be balanced, A sample solution can be carried out and potential measurement standard solution. A.7.3.4 ordinate with the electrode potential value, quality 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 w2 and its value in mg/kg according to formula (A.5) Calculated. 2 10- × = m mw (A.5) Where. Numerical quality test solution m1-- isolated from the working curve of fluorine in milligrams (mg); Numerical m-- sample mass, expressed 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.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 of water is dissolved, add 45 mL hydrochloric acid solution, then dilute hydrochloric acid or dilute ammonia water to adjust the pH to 3.5, Diluted with water to 100 mL. A.8.1.3 saturated hydrogen sulphide water (using now). 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. Weigh 30 g of ammonium sulfate [(NH4) 2SO4], dissolved in water and add water to 100 mL. A.9.1.4 ammonium citrate solution. 250 g/L; Weigh 25 g of ammonium citrate, dissolved in water and add water to 100 mL. A.9.1.5 diethyl dithiocarbamate (DDTC) solution. 50 g/L; Weigh 5 g diethyl dithiocarbamate, dissolved in water and add water to 100 mL. 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 lead 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, 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 From yellow to blue, add 10 mL of ammonium sulfate solution, 10 mL diethyl dithiocarbamate (DDTC) solution, shake. Place 5 min About adding 10mL 4- methyl-2-pentanone (MIBK), shaken vigorously extracted 1 min, after standing layer, the aqueous layer was discarded, 4- methyl-2- Amyl ketone (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 solutions Pipette respectively lead standard solution 0.00 mL, 1.00 mL, 2.00 mL, 4.00 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 nm at Set the standard solution, the absorbance of the 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.9.4 Calculation Results Lead content of lead (Pb) mass fraction w3 and its value in mg/kg according to formula (A.6) Calculated. 3 10- × - = mm w (A.6) Where. Numerical test solution quality lead m1-- isolated from the working curve, in milligr......
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