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GB 25560-2010 English PDF

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GB 25560-2010: National food safety standards of food additive potassium dihydrogen phosphate
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Basic data

Standard ID GB 25560-2010 (GB25560-2010)
Description (Translated English) National food safety standards of food additive potassium dihydrogen phosphate
Sector / Industry National Standard
Classification of Chinese Standard X42
Classification of International Standard 67.220.20
Word Count Estimation 12,185
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 as raw materials prepared food additive potassium dihydrogen phosphate.

GB 25560-2010: National food safety standards of food additive potassium dihydrogen phosphate

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National food safety standards of food additive potassium dihydrogen phosphate National Food Safety Standard Food additive potassium 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 potassium dihydrogen phosphate

1 Scope

This standard applies to thermal phosphoric acid and potassium hydroxide as raw materials obtained food additive potassium dihydrogen 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 KH2PO4 3.2 relative molecular mass 136.09 (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. 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 Potassium dihydrogen phosphate (KH2PO4) (dry basis), w /% ≥ 98.0 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) ≤ 2 Appendix A A.8 Fluorides (as F)/(mg/kg) ≤ 10 Appendix A A.9 pH (10g/L solution) 4.2 ~ 4.7 A.10 Appendix A Loss on drying, w /% ≤ 1.0 Appendix A A.11

Appendix A

(Normative) Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, be careful when operating! As should be immediately splashed on the skin Rinse with plenty of water, severe cases should be treated immediately. Test used in the flammable and should not use an open flame during operation. A.2 General Provisions The standard test methods used in the reagents and water, did not indicate when the other 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 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 nitric acid solution or aqueous ammonia solution liquid. A.3.2.2 Identification of potassium ions 1 g sample was weighed, add 20mL of water to dissolve. 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 viewed with cobalt glass purple. A.4 Determination of potassium 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, Weigh, calculate the content of potassium dihydrogen phosphate. 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 at 105 ℃ ± 2 ℃ electric oven drying 4h sample of about 1.0 g, accurate to 0.000 2 g, placed in 100mL beaker, Water was added to dissolve 50mL, transferred to 250 mL volumetric flask, dilute with water to the mark. 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 treated in the same sample at the same time. A.4.1.4.3 Determination Pipette with a pipette 10.00mL test solution and the blank test solution were placed in 250mL beaker, add 10mL nitric acid solution, Add water to a total volume of about 100 mL, covered with a watch glass, heat to boil 5 min. Cooling the material to the beaker reaches 75 ℃ ± 5 ℃, 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 supernatant filtered decanter Method precipitate was washed with washing 6 times with water to about 30 mL, the precipitate was finally transferred to a glass filter crucible sand, the precipitate was washed with water 4 times. The glass sand crucible together with precipitation placed 180 ℃ ± 5 ℃ electric oven, the timing when the temperature is stable from dried 45 min. Remove coolish After placed in a desiccator, cooled to room temperature, and weighed. A.4.1.5 Calculation Results Potassium dihydrogen phosphate content of potassium dihydrogen phosphate (KH2PO4) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated. () 025 010 0615.0) (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); 0.0615-- quinoline phosphomolybdate converted into potassium dihydrogen phosphate coefficients. Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results is not more than 0.3% absolute difference. A.4.2 acid-base titration A.4.2.1 Method summary In the sample accurately an excess of hydrochloric acid standard titration solution of sodium hydroxide standard solution titrate excess hydrochloric acid standard titration solution Solution to pH meter indicating jump point, according to the consumption of sodium hydroxide standard titration solution, potassium 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 in advance at 105 ℃ ± 2 ℃ electric oven drying 4h about 5g sample, accurate to 0.000 2g, placed in a 250mL Beaker, 40.00mL standard titration solution of hydrochloric acid and 50mL water. Then placed on a magnetic stirrer, into the mixing rotor and stir until The sample is completely dissolved. Then the pH meter calibrated electrodes placed in the test solution, standard titration with sodium hydroxide solution to titrate excess salt Acid standard titration solution until pH≈4.0 appear jump point, recording titration readings (V), calculate the sample consumption hydrochloric acid standard titration solution body Product (V1). Standard titration with sodium hydroxide solution and continue titration until pH≈8.8 appear jump point, recording titration readings, calculated in the two projections Hop sodium hydroxide standard titration between (pH≈4.0 to pH≈8.8) titration volume of solution consumed (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). Potassium dihydrogen phosphate with potassium dihydrogen phosphate (KH2PO4) mass fraction w1 and its value is expressed in%, according to formula (A.3) Calculated. 010) ( 1 ××× - = McVcVw (A.3) Where. Numerical hydrochloric acid standard titration V1-- titration appears to pH≈4 jump point solution consumed 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-- potassium dihydrogen phosphate (of KH2PO4) the molar mass of the units of grams per mole (g/mol) (M = 136.09). Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results is not more than 0.2% absolute difference. 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 105 ℃ ± 2 ℃ electric oven drying to constant quality glass sand filtration crucible, with 200 mL of hot water 10 minutes wash water insolubles. will Sand glass crucible together with water-insoluble substance placed 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 0.002%. 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 the same sample at the same time Management. 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 Dilute with water to volume, and mix. Dry filtration medium speed filter paper, discard the first 20mL solution, with a pipette, take 20mL test solution was placed in 50mL Colorimetric tube. Add 1 drop of phenolphthalein indicator solution (10g/L), with sodium hydroxide solution (40g/L) solution was adjusted to neutral with water to a total volume of About 30mL, according to GB/T 5009.74-2003 Determination of Chapter 6. Standard colorimetric solution preparation. Using a pipette 1 mL of lead standard solution [1 mL solution containing lead (Pb) 0.010mg], and the sample at the same time The same treatment. 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) 0.010 mg; 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 It weighs about 10g sample, accurate to 0.01g, placed in 150mL beaker. Add water 30mL and 2mL of hydrochloric acid to dissolve the sample. Heat and cook Boiling 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 liquid separation Funnel, diluted with water to about 150mL. Add 2mL Pyrrolidine dithiocarbamate (The APDC) solution, and mixed. Extracted with chloroform Taken twice added 20 mL, the extract (i.e., organic phase) was collected in a clean 50mL beaker, evaporated to near dryness steam bath, add 3mL nitrate Acid, heat nearly dry. Then add 0.5mL of nitric acid and 10mL deionized water, heated to the remaining 3 mL ~ 5mL. The extract was set to transfer the nitrified In 10mL volumetric flask, dilute to the mark, shake. 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 "heated to boiling A few minutes, the solution is cooled, diluted to 100 mL transfer nitrified placed 10 mL volumetric flask, dilute with water to the mark. " A.8.3.4 Determination A.8.3.4.1 instrument conditions. resonance line of 283.3 nm; slit 0.7 nm; air - acetylene flame. A.8.3.4.2 Determination. The test solution, standard solution to import atomic absorption spectrophotometer, zero blank test solution, the test solution Absorption value was not 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) was dissolved in 800 mL In 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 1.00 mL of fluoride standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark with water, shake uniform. This solution was formulated with time. 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 the negative terminal of a saturated calomel electrode and the measuring instrument is connected to the positive terminal of the electrode inserted into a plastic cup filled with water, After electromagnetic stirring (polyethylene rotor), read the value of the equilibrium potential, the replacement of 2 to 3 times the water until the potential reaches the electrode manual regulation After the predetermined potential value, potential measurement can be carried out. A.9.3.2 draw the curve Pipette solution 1.00mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00mL and 10.00 mL of fluoride standard solution, were placed 6 A 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 Blue, and then the nitric acid solution to adjust the solution as a yellow, diluted with 20mL of buffer solution with water to the mark. The solution was poured into clean, Dried 50 mL beaker placed on a magnetic stirrer, stirring into the insert fluoride electrode and a saturated calomel electrode selection, open stir Mix, and record the potential value at equilibrium. In logarithm fluoride content as abscissa, the corresponding potential value of the vertical axis, draw the working curve. A.9.3.3 Determination It weighs about 3 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 "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 opposition Number obtained fluorine ion mass. A.9.4 Calculation Results Fluoride content of fluorine (F) mass fraction w3 and its value in mg/kg according to 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 greater than 2 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. With the pH has been corrected 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 ℃ ± 2 ℃ weighing bottle Weigh about 5g samples, accurate to 0.000 2g, placed power of 105 ℃ ± 2 ℃ Thermal thermostatic oven, the drying 4h, the weighing bottle was cooled to room temperature in a desiccator, and weigh. 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); 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 0.01%.

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