GB 25564-2010 English PDF

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GB 25564-2010: The national food safety standards of food additives sodium dihydrogen phosphate
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Basic data

Standard ID: GB 25564-2010 (GB25564-2010)
Description (Translated English): The national food safety standards of food additives sodium dihydrogen phosphate
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Classification of International Standard: 67.220.20
Word Count Estimation: 12,186
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 caustic sodium hydroxide or sodium carbonate prepared food additive sodium dihydrogen phosphate.

GB 25564-2010: The national food safety standards of food additives sodium dihydrogen phosphate

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The national food safety standards of food additives sodium dihydrogen phosphate National Food Safety Standard Food additive, sodium dihydrogen 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 additive, sodium dihydrogen phosphate

1 Scope

This standard applies to thermal phosphoric acid and caustic sodium hydroxide or sodium carbonate prepared food additive sodium dihydrogen phosphate.

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 NaH2PO4 • nH2O (n = 0, n = 1, n = 2) 3.2 relative molecular mass 119.98 (n = 0) (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 texture. State organization crystalline powder or granules 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Sodium dihydrogen phosphate (NaH2PO4) (dry basis), w /% 98.0 ~ 103.0 Appendix A A.4 Water-insoluble, w /% ≤ 0.2 A.5 in Appendix A Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.6 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.7 Lead (Pb)/(mg/kg) ≤ 4 Appendix A A.8 Table 2. Physical and chemical indicators (cont.) Fluorides (as F)/(mg/kg) ≤ 50 Appendix A A.9 pH (10g/L solution) 4.1 ~ 4.7 A.10 Appendix A Loss on drying (NaH2PO4), w /% ≤ 2.0 Appendix A A.11 (NaH2PO4 · H2O), w /% 10.0 ~ 15.0 (NaH2PO4 · 2H2O), w /% 20.0 ~ 25.0

Appendix A

(Normative) Testing method A.1 Safety Tips Chemical reagents part of this standard test method used in corrosive, the operation should be careful. As splashed on the skin, immediately wash with water. In 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 in Regulation Given three water. Used in the test standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according to HG/T 3696.1, 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 ammonia solution. 23. A.3.1.2 nitric acid solution. 18. A.3.1.3 silver nitrate solution. 17 g/L. A.3.2 Analysis step A.3.2.1 Identification of phosphate 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.3.2.2 Identification of sodium ions Weigh 1 g sample, add water to dissolve 20mL. Platinum wire ring dipped in hydrochloric acid, in a colorless flame to burn. And then dipped in the test solution on the flame Combustion, the flame should be bright yellow. A.4 Determination of sodium dihydrogen phosphate A.4.1 gravimetric method (Arbitration Act) A.4.1.1 Method summary In acidic medium, the root and the phosphoric acid test solution was added a solution of Quimociac quinoline phosphomolybdate formed precipitate was collected by filtration, dried, Weighing, sodium dihydrogen phosphate content was calculated. A.4.1.2 Reagents and materials A.4.1.2.1 nitric acid solution. 11. A.4.1.2.2 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 ℃. A.4.1.4 analysis step A.4.1.4.1 Preparation of test solution Weigh 105 ℃ drying 4h about 1.0 g samples, accurate to 0.000 2 g, placed in 100mL beaker, add water to dissolve 50mL, shift Into a 250 mL volumetric flask, dilute to the mark, shake. Preparation A.4.1.4.2 blank test solution Except that no sample addition, the same amount of reagent preparation and join other test solution, and the sample subjected to the same treatment at the same time. A.4.1.4.3 Determination Pipette Pipette 10mL test solution and the blank test solution were placed in 250mL beaker, add 10mL nitric acid solution, add water to The total volume of about 100 mL, covered with a watch glass heated to boiling for 5 min. After cooling, the cooling process (temperature of the solution at about 75 ℃) was added 50mL Quimociac solution (addition of the reagents and the heating process can not use open flame can not be stirred, so as not to clot). Cooling, during cooling Stirring for 3 to 4 times, with pre-drying to a constant mass of glass sand filtration crucible at 180 ℃ ± 5 ℃. First filtered supernatant, decantation The precipitate was washed with washing 6 times, each time with water of about 30 mL, the precipitate was finally transferred to a glass filter crucible sand, the precipitate was washed with water 4 times, Sand glass crucible placed together with electric oven in precipitation, temperature stable from time, at 180 ℃ ± 5 ℃ dried 45 min, remove the coolish After cooling to room temperature, placed in a desiccator, and weigh. A.4.1.5 Calculation Results Sodium dihydrogen phosphate content of sodium dihydrogen phosphate (NaH2PO4) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated. () 025 010 05422.0) (21 1 ×× × - = mmw (A.1) Where. M1-- value quality test solution to generate quinoline phosphomolybdate precipitate in grams (g); Numerical quality m2-- blank test solutions generate quinoline phosphomolybdate precipitate in grams (g); m-- sample mass value in grams (g); 0.05422-- Quinoline phosphomolybdate terms of the coefficients of sodium dihydrogen phosphate. 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.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 Solution to pH meter indicating jump point, according to the consumption of sodium hydroxide standard titration solution, sodium dihydrogen 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 electromagnetic stirrer. stirring with a rotor. A.4.2.4 analysis step Weigh the sample in advance at 105 ℃ drying 4h about 5g, accurate to 0.0002g, placed in a 250mL beaker, add salt 40.0mL Acid standard titration solution and 50mL water. Then placed on a magnetic stirrer, stirring into the rotor, and stir until the sample is completely dissolved. Then calibrated pH meter electrodes registration into the test solution, titrated with sodium hydroxide solution to titrate the excess standard hydrochloric acid standard titration solution until pH≈4.0 Appear jump point, recording titration readings (V), calculate the sample consumption hydrochloric acid standard titration solution volume (V1). Standard titration with sodium hydroxide solution Continue titration solution appears to pH≈8.8 jump point, recording titration readings, calculate the titration jump in both points (pH≈4.0 ~ pH≈8.8) between The volume of consumption of sodium hydroxide standard titration solution (V2). A.4.2.5 Calculation Results Sample consumption hydrochloric acid standard titrant volume (V1) according to formula (A.2) Calculated. twenty one 0.40 VccV - = (A.2) Where. Numerical consumed V-- titration jump point appears to pH≈4.0 sodium hydroxide standard titration solution volume in milliliters (mL); The actual value of the concentration of hydrochloric acid standard titration solution c1-- units of moles per liter (mol/L); The actual value of c2-- concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L). Sodium dihydrogen phosphate, sodium dihydrogen phosphate (NaH2PO4) mass fraction w1 and its value is expressed in%, according to formula (A.3) Calculated. 010) ( 1 ××× - = McVcVw (A.3) Where. When V1-- titration appears to pH≈4.0 jump point, the value of hydrochloric acid standard titration solution consumed by the sample volume in milliliters (mL); V2 - sodium hydroxide standard titration value between pH≈4.0 ~ pH≈8.8 titration solution consumed volume in milliliters (mL); Accurate c1-- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L); The exact value c2-- sodium hydroxide standard titration solution concentration, expressed in moles per liter (mol/L); m-- sample mass value in grams (g); Numerical M-- sodium dihydrogen phosphate (of NaH2PO4) molar mass in grams per mole (g/mol) (M = 119.98). 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 Determination of insoluble matter A.5.1 Instruments and Equipment A.5.1.1 sintered glass crucible. filter plate pore size of 5 μm ~ 15 μm. A.5.1.2 electric oven. the temperature can be controlled at 105 ℃ ± 2 ℃. A.5.2 Analysis step Weigh approximately 10 g samples, accurate to 0.01 g, placed in 400 mL beaker, add 100 mL of water and heated to boiling, hot with advance at 105 ℃ Drying to constant quality glass sand filtration crucible, with 200 mL of hot water 10 minutes wash water insolubles. The glass sand crucible was placed together with water-insoluble 105 ℃ ± 2 ℃ electric oven, and bake until constant mass. A.5.3 Calculation Results Water-insoluble mass fraction w2 and its value is expressed in%, according to formula (A.4) Calculated. 0122 × - = m mmw (A.4) Where. Numerical m2-- water insoluble sand and glass crucible mass in grams (g); Numerical m1-- sintered 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 0.02%. A.6 Determination of Arsenic Weigh 0.50g ± 0.01g sample was placed in 100mL beaker, add 20 mL of water and 10 mL hydrochloric acid solution (11), heated to dissolve, All transferred to measure arsenic bottle, add water to a total volume of about 40mL, measured according to GB/T 5009.76-2003 Chapter 11 provisions. Limits formulated solution. Pipette 1.50 mL of arsenic standard solution [1 mL solution of arsenic (As) 1.0μg], and treated in the same sample at the same time. A.7 Determination of Heavy Metals Weigh 5.00g ± 0.01g sample was placed in 100mL beaker, add 80 mL of water, heated to dissolve moved to 100 mL volumetric flask with water Dilute to volume, and mix. Dry filtration medium speed filter paper, discard the first 20mL solution, with a pipette, take 20.00mL test solution was placed in 50mL Colorimetric tube. Using hydrochloric acid solution (12) to acidic solution (pH≈3 precision test paper), add water to a total volume of about 30mL, According to GB/T 5009.74-2003 Determination of Chapter 6. Preparation of standard colorimetric solution. pipette Pipette 1 mL of lead standard solution [1 mL solution containing lead (Pb) 10 μg], and the same sample at the same time deal with. A.8 Determination of Lead A.8.1 Reagents and materials A.8.1.1 hydrochloric acid. A.8.1.2 nitrate. A.8.1.3 sodium hydroxide solution.200g/L. A.8.1.4 chloroform. A.8.1.5 Pyrrolidine dithiocarbamate (The APDC) solution. 20g/L. Filtered before use. A.8.1.6 Lead standard solution. 1 mL solution containing lead (Pb) 10 μg; Pipette Pipette 1.00mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark. A.8.1.7 two water. in line with GB/T 6682-2008 requirements. A.8.2 Instruments and Equipment Atomic absorption spectrophotometer. A.8.3 Analysis step A.8.3.1 Preparation of test solution Weigh 10.0g ± 0.01g sample in 150mL beaker. Add 30mL water, add 2mL of hydrochloric acid to dissolve the sample. Heat to boil a few minutes, Cooled, diluted to 100mL, with sodium hydroxide solution to adjust the pH to 1.0 to 1.5. The entire solution was transferred to a 250mL separatory funnel, washed with water Diluted to about 150mL. Add 2mL Pyrrolidine dithiocarbamate (The APDC) solution, and mixed. Extracted with chloroform twice plus Into 20 mL, the extract (ie, organic phase) was collected in a clean 50mL beaker, steam bath and evaporated nearly dry, add 3mL nitric acid heated nearly dry. However After the addition of nitric acid 0.5mL and 10mL water, heated to the remaining 3 mL ~ 5mL. The extract was transferred nitrified placed 10mL volumetric flask, dilute with water Release to the mark. A.8.3.2 Preparation of the blank test solution Take 30 mL water were placed in a 150 mL beaker, add 1 mL of hydrochloric acid. The following operation is the same in A.8.3.1 "boil a few minutes heating, cooling, The extract was diluted to 100 mL transfer nitrified placed 10 mL volumetric flask, diluted with water to the mark. " A.8.3.3 Preparation of standard solutions Pipette 4.00 mL of lead standard solution was placed in a 150 mL beaker, add 1 mL of hydrochloric acid. The following operation is the same A.8.3.1 in "a few heated to boiling Minutes, cooled, diluted with 100 mL transferred to extract nitrified placed 10 mL volumetric flask, diluted with water to the mark. " A.8.3.4 Determination a) instrument conditions. resonance line of 283.3 nm; slit 0.7 nm; air - acetylene flame. b) Determination. The test solution, standard solution to import atomic absorption spectrophotometer, zero blank test solution, the test solution suction Closing value can not be higher than the standard solution absorbance. A.9 Determination of fluoride A.9.1 Reagents and materials A.9.1.1 hydrochloric acid solution. 14. A.9.1.2 nitric acid solution. 115. A.9.1.3 sodium hydroxide solution. 100 g/L. A.9.1.4 buffer solution. 270 g sodium citrate dihydrate (Na3C6H5O7 · 2H2O) and 24 g of citric acid (C6H5O7 · 2H2O) in 800 mL of water, then diluted with water to 1 000 mL. A.9.1.5 fluoride standard solution. 1 mL solution of fluorine (F) 0.010 mg. Pipette Pipette 1 mL of fluoride standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark, Shake well. This solution is using now. A.9.1.6 bromocresol green indicator solution. 1 g/L. A.9.2 Instruments and Equipment A.9.2.1 fluoride ion selective electrode. A.9.2.2 saturated calomel electrode. A.9.2.3 potentiometer. A.9.3 Analysis step A.9.3.1 Instrument adjustment The fluoride ion selective electrode and a saturated calomel electrode and the negative terminal of the measuring instrument connected to the positive terminal of the electrode insert a plastic cup filled with water, in After the electromagnetic stirring (polyethylene rotor), read the value of the equilibrium potential, the replacement of 2 to 3 times the water until the electrode potential reaches the specified in the instructions After the potential value, potential measurement can be carried out. A.9.3.2 draw the curve Pipette 1.00mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00mL, 10.00mL fluoride standard solution, were placed in six 50mL Volumetric flask, add 1 mL of hydrochloric acid solution and 5 drops of buffer solution, 2 drops of bromocresol green indicator solution. The solution was adjusted with sodium hydroxide solution to blue, and then Yellow solution was adjusted with nitric acid solution, diluted with 20mL of buffer solution with water to the mark. The solution was poured into a clean, dry 50 mL Beaker placed on a magnetic stirrer, stirring into the insert fluoride electrode and a saturated calomel electrode selection, the stirrer, recording balance Potential value. In logarithm fluoride content as abscissa, the corresponding potential value of the vertical axis, draw the working curve. A.9.3.3 Determination Weigh approximately 1 g samples, accurate to 0.000 2 g, placed in 50 mL volumetric flask, add 10 mL of water, following in A.9.3.2 self "plus 1 mL hydrochloric acid solution "to" record potential value at equilibrium. "Find out the number corresponding to the content of fluoride ions from the working curve, seeking antilog Obtained fluorine ion mass. A.9.4 Calculation Results Fluoride content of fluorine (F) mass fraction w3 and its value in mg/kg expressed by the formula (A.5) Calculated. 3 10- × = m mw (A.5) Where. Numerical m1-- test solution fluoride ion 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 5 mg/kg. A.10 pH measurement of A.10.1 instruments and equipment pH meter. Indexing is 0.02. A.10.2 Analysis steps Weigh 1.00g ± 0.01g sample, placed in 100 mL volumetric flask, dissolved in water and diluted to the mark. It has been corrected with acidity Measured pH of the solution. A.11 Determination of loss on drying A.11.1 instruments and equipment Electric oven. the temperature can be controlled at 105 ℃ ± 2 ℃. A.11.2 Analysis steps Use has been dried to a constant mass of 105 ℃ weighing bottle Weigh about 5g samples, accurate to 0.000 2g, first placed in an electric constant of 60 ℃ ± 2 ℃ Temperature oven and dried 1h, then placed in 105 ℃ ± 2 ℃ the electric oven, the drying 4h. The weighing bottle placed in the dryer to cool To room temperature, and weighed. A.11.3 Calculation Results Loss on drying mass fraction w4 and its value is expressed in%, according to formula (A.6) Calculated. 014 × - = m mmw (A.6) Where. Value after m1-- dried sample mass, expressed 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 0.2%. ......

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