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GB 25561-2010: The national food safety standards of food additives dipotassium hydrogen phosphate
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The national food safety standards of food additives dipotassium hydrogen phosphate
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Basic data | Standard ID | GB 25561-2010 (GB25561-2010) | | Description (Translated English) | The national food safety standards of food additives dipotassium hydrogen phosphate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 12,173 | | 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 for raw materials for food additives dipotassium hydrogen phosphate. | GB 25561-2010: The national food safety standards of food additives dipotassium hydrogen phosphate
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The national food safety standards of food additives dipotassium hydrogen phosphate
National Food Safety Standard
Food additives dipotassium hydrogen
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 dipotassium hydrogen
1 Scope
This standard applies to thermal phosphoric acid and potassium hydroxide as raw materials obtained food additive potassium phosphate dibasic.
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
K2HPO4
3.2 relative molecular mass
174.18 (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. 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
Dipotassium hydrogen phosphate (K2HPO4) (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
Table 2. Physical and chemical indicators (cont.)
pH (10g/L solution) 9.0 ± 0.4 A.10 Appendix A
Loss on drying, w /% ≤ 2.0 Appendix A A.11
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
Or treatment.
A.2 General Provisions
Test methods for this standard reagents and water, did not indicate when the 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 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 the test solution on the flame
Combustion, the flame should be viewed with cobalt glass purple.
A.4 Determination of potassium phosphate dibasic
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,
Weighed, calculated dipotassium hydrogen content.
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 about 1.0 g samples, 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
But without addition of the sample, the other operations and the same amount of reagent preparation is added and the test solution, and treated in the same sample at the same time.
A.4.1.4.3 Determination
Pipette pipette 15.00mL test solution and the blank test solution were placed in 250mL beaker, add 10mL nitric acid solution was added
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 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. will
After the sand glass crucible placed in an electric oven, along with precipitation temperature stable from the timing, at 180 ℃ ± 5 ℃ dried 45 min, remove the coolish, dry place
Dryer cooled to room temperature and weighed.
A.4.1.5 Calculation Results
Dipotassium phosphate content of potassium phosphate dibasic (K2HPO4) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated.
() 025 015
07871.0) (21
1 ××
× - =
mmw (A.1)
Where.
m1-- test solution to generate quinoline phosphomolybdate precipitate mass value in grams (g);
m2-- blank test solution to generate mass values quinoline phosphomolybdate precipitate in grams (g);
Numerical m-- sample mass, expressed in grams (g);
0.07871-- Quinoline phosphomolybdate terms of dipotassium hydrogen 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%.
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, calculated dibasic potassium phosphate content.
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 ℃ drying 4h of potassium phosphate dibasic sample of about 5g, accurate to 0.000 2g, placed in a 250mL beaker, add
Into 40.0mL standard titration solution of hydrochloric acid and 50mL water. Then placed on a magnetic stirrer, stirring into the rotor, and stir until the sample is completely dissolved.
Then the pH meter calibrated electrodes placed in 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 volume of sample consumption hydrochloric acid standard titration solution (V1). Hydroxide
Sodium standard titration solution and continue titration until pH≈8.8 appear jump point, recording titration readings, calculated in the two jump points (pH≈4.0 to pH≈
Volume 8.8) between the consumption of sodium hydroxide standard titration 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).
When V1c1 equal to or less than V2c2, dipotassium hydrogen phosphate, dipotassium hydrogen phosphate (K2HPO4) mass fraction w1 and its value is expressed in%
According to the formula (A.3) Calculated.
1 ××× =
McVw (A.3)
When V1c1 more than V2c2, dipotassium hydrogen phosphate, dipotassium hydrogen phosphate (K2HPO4) mass fraction w1 and its value is expressed in%, according to public
Formula (A.4) Calculated.
010) 2- (
1 ××× - =
McVcVw (A.4)
Where.
When V1-- titration appears to pH≈4 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);
Numerical m-- sample mass, expressed in grams (g);
Numerical dipotassium hydrogen M-- (K2HPO4 on) the molar mass of the units of grams per mole (g/mol) (M = 174.18).
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 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 ℃ drying to constant quality glass sand filtration crucible, with 200 mL of hot water 10 minutes wash water insolubles. The crucible together with water glass sand
Insolubles were placed in 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.5) Calculated.
0122 × - = m
mmw (A.5)
Where.
Numerical m2-- quality water insoluble sand and glass crucible, in grams (g);
Numerical m1-- quality glass sand crucible 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 0.02%.
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, according to GB/T 5009.76-2003 provisions of Chapter 11 of the operation.
Limits formulated solution. Pipette 1.50 mL of arsenic standard solution [1 mL solution of arsenic (As) 1μg], 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. Add 1 drop of phenolphthalein indicator solution (10g/L), with sodium hydroxide solution (40g/L) was adjusted to neutral solution, add water to a total volume of about
30mL, according to GB/T 5009.74-2003 Chapter 6 operation.
Color than the standard preparation solution. pipette Pipette 1.00mL lead standard solution [1 mL solution containing lead (Pb) 0.010 mg], and the same sample
When 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 Pipette 1.00mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark,
Shake well.
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 30mL of water and 1mL hydrochloric acid to dissolve the sample, and then the excess 1mL
Hydrochloric acid to ensure that the sample is dissolved. Heated to boiling for a few minutes, cooled, diluted to 100mL, with sodium hydroxide solution to adjust the pH to 1.0 to 1.5. The solution
All were transferred to a 250mL separating funnel, diluted with water to about 150mL. 2mLAPDC solution was added and mixed. Two extracted with chloroform
Times added to 20 mL, the extract (i.e., organic phase) was collected in a clean 50mL beaker, evaporated to near dryness steam bath, add 3mL nitric acid, plus
Nearly dry heat. Then add 0.5mL nitric acid and 10mL water, heated to the remaining 3 mL ~ 5mL. The extract was transferred into 10mL capacity nitrified
Bottle diluted with water 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 2.00 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
Diluted minutes, cooled with water to extract 100 mL transfer nitrified placed 10 mL volumetric flask, dilute 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 1.00 mL of fluoride standard solution according to HG/T 3696.2 formulated into 100 mL volumetric flask, dilute to the mark with water
Degree, shake. 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 draw the curve
Pipette 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL fluoride standard solution, were placed in six 50mL capacity
Flask, add 1 mL of hydrochloric acid solution and 5 drops of buffer solution, 2 drops of bromocresol green indicator solution. Adjusted with sodium hydroxide solution to a blue solution, and then
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 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.9.3.2 Determination
Weigh about 3.0 g samples, accurate to 0.000 2 g, placed in 50 mL volumetric flask, add 10 mL of water, following in A.9.3.1 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 was evaluated antilog
To fluorine ion mass.
A.9.4 Calculation Results
Fluorine content of fluorine (F) mass fraction w3 and its value in mg/kg according to formula (A.6) Calculated.
3 10- × = m
mw (A.6)
Where.
Numerical m1-- test solution fluoride ion mass, 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 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. 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 ℃ ± 2 ℃ weighing bottle Weigh about 5g samples, accurate to 0.0002g, placed power of 105 ℃ ± 2 ℃
Hot thermostatic oven dried to constant mass.
A.11.3 Calculation Results
Loss on drying mass fraction w4 and its value is expressed in%, according to formula (A.7) calculated as follows.
014 × - = m
mmw (A.7)
Where.
Value quality m1-- after drying the sample 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 0.02%.
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