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GB 25569-2010: The national food safety standards of food additives ammonium dihydrogen phosphate
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The national food safety standards of food additives ammonium dihydrogen phosphate
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Basic data | Standard ID | GB 25569-2010 (GB25569-2010) | | Description (Translated English) | The national food safety standards of food additives ammonium dihydrogen phosphate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 12,110 | | 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 ammonia as raw food additive ammonium dihydrogen phosphate. | GB 25569-2010: The national food safety standards of food additives ammonium dihydrogen phosphate
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The national food safety standards of food additives ammonium dihydrogen phosphate
National Food Safety Standard
Food Additives ammonium 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 Additives ammonium dihydrogen phosphate
1 Scope
This standard applies to thermal phosphoric acid and ammonia as raw materials, food additives, ammonium 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
NH4H2PO4
3.2 relative molecular mass
115.02 (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 was observed under natural light
Color and texture. 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
Ammonium dihydrogen phosphate (in NH4H2PO4 dollars), w /% 96.0 ~ 102.0 Appendix A A.4
Fluorides (as F)/(mg/kg) ≤ 10 Appendix A A.5
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
pH (10g/L aqueous solution) 4.3 to 5.0 A.9 Appendix A
Appendix A
(Normative)
Testing method
A.1 Warning
Reagents The standard test methods used for toxic or corrosive, be careful when operating! Should immediately splashed on the skin, such as
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 in
Three water regulations. 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 nitric acid solution. 18.
A.3.1.2 ammonia solution. 11.
A.3.1.3 sodium hydroxide solution. 40g/L.
A.3.1.4 silver nitrate solution. 17g/L.
A.3.1.5 red litmus paper.
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 ammonium ions
Weigh about 0.5g sample with sodium hydroxide solution to dissolve the sample, releasing ammonia, make moist red litmus paper blue. Heating can be
Promote decomposition.
A.4 Determination of ammonium dihydrogen phosphate
A.4.1 gravimetric method (Arbitration Act)
A.4.1.1 Method summary
In acidic medium, Quimociac with the test solution phosphate reaction quinoline phosphomolybdate precipitate, the precipitate was filtered, dried, weighed,
Calculation of ammonium dihydrogen phosphate content of the sample.
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 sand core glass crucible. pore size 5μm ~ 15μm.
A.4.1.3.2 electric oven. the temperature can be controlled at 180 ℃ ± 2 ℃.
A.4.1.4 analysis step
A.4.1.4.1 Preparation of test solution
Weigh about 1g sample, accurate to 0.0002g. Placed 100 mL beaker, add a small amount of water to dissolve. Transferred to 500 mL volumetric flask with water
Diluted to the mark, shake, dry filter (discarded first filtrate 20mL).
A.4.1.4.2 Determination
Pipette 20.00 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, was added
50 mL Quimociac solution, cover the surface of the dish and heated in a water bath until the material in the beaker reaches 75 ℃ ± 5 ℃ (in a fume hood), Paul
Warm 30s (in addition of the reagents and the heating process can not use open flame can not be stirred, so as not to clot). Cooling the mixture was stirred in the cooling process 3
To 4 times, with pre-drying 45min glass sand core filtration crucible at 180 ℃ ± 2 ℃. First supernatant was filtered, washing with decantation
The precipitate was washed six times, each time with water of about 30 mL, the precipitate was finally transferred to a sintered glass crucible was filtered, the precipitate was washed with water 4 times. The glass
Sand core crucible together with precipitation into electric oven, the temperature was stabilized from the beginning of time, at 180 ℃ ± 2 ℃ dried under 45min. Remove coolish
After cooling to room temperature, placed in a desiccator, and weighed.
Meanwhile blank test, but without addition of the sample, the other reagent type and the same amount of blank test solution was added, and the test
Treated in the same test solution.
A.4.1.5 Calculation Results
Ammonium dihydrogen phosphate content of ammonium dihydrogen phosphate (NH4H2PO4) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated.
) 50020 (
05198.0) (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);
Numerical m-- sample mass, expressed in grams (g);
0.05198-- quinoline phosphomolybdate converted into diammonium phosphate coefficients.
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.4.2 volumetric method
A.4.2.1 Method summary
After the dissolution of the sample solution was titrated with sodium hydroxide standard titration, pH meter to indicate the end, based on the volume of consumption of sodium hydroxide standard titration solution
Plot, calculate the content of ammonium dihydrogen phosphate.
A.4.2.2 Reagents and materials
A.4.2.2.1 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L.
A.4.2.2.2 carbon dioxide-free water.
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 about 0.5g sample to the nearest 0.000 2g, placed 150 mL beaker. No carbon dioxide was added 50 mL of water, placed in an electromagnetic
Agitator, into the mixing rotor and stir until the sample is completely dissolved. The pH meter is calibrated electrode into the test solution, with sodium hydroxide
Standard titration solution was titrated to pH 8.0, the recording volume consumed sodium hydroxide standard titration solution.
A.4.2.5 Calculation Results
Ammonium dihydrogen phosphate content of ammonium dihydrogen phosphate (NH4H2PO4) mass fraction w1 and its value is expressed in%, according to formula (A.2) Calculated.
010001 × = m
cVMw (A.2)
Where.
Numerical sodium hydroxide standard titration solution consumed V-- titration solution volume in milliliters (mL);
The exact concentration of sodium hydroxide standard titration solution c-- value in units of moles per liter (mol/L);
Numerical m-- sample mass, expressed in grams (g);
Numerical M-- ammonium dihydrogen phosphate (NH4H2PO4) molar mass in grams per mole (g/moL) (M = 115.0).
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.5 Determination of fluoride
A.5.1 Reagents and materials
A.5.1.1 hydrochloric acid solution. 111.
A.5.1.2 sodium acetate solution. c (CH3COONa • 3H2O) ≈3mol/L;
Weigh 204g of sodium acetate (CH3COONa • 3H2O), was dissolved in 300mL of water, add a solution of acetic acid (116) adjusting the pH to 7.0, add
Diluted with water to 500mL.
A.5.1.3 sodium citrate solution. c (Na3C6H5O7 • 2H2O) ≈0.75mol/L;
Weigh 110g sodium citrate (Na3C6H5O7 • 2H2O) was dissolved in 300mL of water, diluted with 14mL of perchloric acid, add water to 500mL.
A.5.1.4 total ionic strength buffers.
Volume mixing sodium acetate and sodium citrate solution, etc., before use this solution formulation.
A.5.1.5 fluoride standard solution. 1mL solution of fluorine (F) 0.001mg;
Pipette Pipette 1mL fluoride standard solution according to HG/T 3696.2 prepared, placed in 1000mL volumetric flask, dilute to the mark,
Shake well. The solution was formulated before use.
A.5.2 Instruments and Equipment
A.5.2.1 fluoride ion selective electrode.
A.5.2.2 saturated calomel electrode.
A.5.2.3 electromagnetic stirrer. with polyethylene rotor.
A.5.2.4 pH meter. dividing the value 0.01.
A.5.3 Analysis step
A.5.3.1 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.5.3.2 Preparation of test solution
Weigh about 1g sample to the nearest 0.01g. A 50mL beaker was added dissolved in water 10mL, transferred to a 50mL volumetric flask, add
Total ionic strength buffer dilution 25mL, 10mL hydrochloric acid solution, add water to the mark. Poured into a plastic beaker 25mL measuring electrode potential.
A.5.3.3 draw the curve
Pipette respectively 1.00mL, 5.00mL, 8.00mL, 10.00mL, 15.00mL fluoride standard solution (equivalent to the fluorine content respectively
0.001mg, 0.005mg, 0.008mg, 0.010mg, 0.015mg) in five 50mL volumetric flask, were added to each flask 25mL
Dilution total ionic strength buffer, 10mL hydrochloric acid solution, add water to the mark. Pour 50mL clean, dry plastic beaker was measured
Electrode potential.
Ordinate the electrode potential, the quality of fluorine (mg) as abscissa, the curve on semi-log graph paper, according to the potential of the sample
Richard curve value on the quality of fluoride ions.
A.5.4 Calculation Results
Fluoride content of fluorine (F) mass fraction w2 and its value in mg/kg according to formula (A.3) Calculated.
2 m
mw = (A.3)
Where.
m1-- potential value based on the measured value of the test solution from the working curve Richard fluorine mass, in milligrams (mg);
m - the value of the sample mass, 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.6 Determination of Arsenic
A.6.1 diethyl dithiocarbamate silver colorimetry (Arbitration Act)
A.6.1.1 Reagents and materials
With GB/T 5009.76-2003 first law diethyl dithiocarbamate silver colorimetry Chapter 3.
A.6.1.2 analysis step
Weigh about 1g sample to the nearest 0.01g. Arsenic occurs put the bottle, add water to about 40mL, add 10mL sulfuric acid solution (11) After the dissolution,
The following press 6.3 GB/T 5009.76-2003 first law "lessons 0,2.00,4.00,6.00,8.00,10.00mL arsenic standard series
The same method should also be treated to the standard curve calibration "operation.
A.6.1.3 Calculation Results
Arsenic content quality of arsenic (As) scores w3 and its value in mg/kg according to formula (A.4) Calculated.
1000) (01
3 m
mm
- = (A.4)
Where.
Numerical quality test solution m1-- isolated from the working curve arsenic, in milligrams (mg);
Numerical quality blank test solution m0-- isolated from the working curve arsenic, in milligrams (mg);
Mass values m-- sample in grams (g).
Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results of absolute difference is not more than 1 mg/kg.
A.6.2 Gutzeit method
A.6.2.1 Reagents and materials
Reagents with GB/T 5009.76-2003 Chapter 9.
A.6.2.2 instruments and equipment
With GB/T 5009.76-2003 Chapter 10.
A.6.2.3 analysis step
Weigh 0.50g ± 0.01g sample was placed in measuring arsenic flask, add 20mL water. The following operation is the same GB/T 5009.76-2003 Chapter 11, "plus
5mL hydrochloric acid must not Gutzeit "deeper than the limits of arsenic.
Limits formulated solution. Pipette 1.50mL arsenic standard solution [1mL solution containing arsenic (As) 0.001mg], the following actions with GB/T 5009.76
Chapter 11 -2003 "plus 5mL hydrochloric acid removed Gutzeit compare." Simultaneously with the sample.
A.7 Determination of Heavy Metals
A.7.1 Reagents and materials
A.7.1.1 hydrochloric acid solution. 11.
A.7.1.2 ammonia solution. 23.
A.7.1.3 acetate buffer solution. pH = 3.5;
Weighed 25.0 g ammonium acetate, add 25 mL of water dissolved, and 45 mL hydrochloric acid solution, aqueous ammonia solution or hydrochloric acid solution and then adjusted to pH 3.5,
Diluted with water to 100 mL.
A.7.1.4 saturated hydrogen sulphide water.
A.7.1.5 Lead standard solution. 1mL solution containing lead (Pb) 0.01mg;
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. The solution was formulated before use.
A.7.2 Instruments and Equipment
Colorimetric tube. 50mL.
A.7.3 Analysis step
Weigh 10.00g ± 0.01g sample was placed in 150mL beaker, add 80mL water, dissolved moved to 100 mL volumetric flask, dilute with water
Release to the mark. Filtered and the filtrate was discarded initial 20mL. Pipette pipette 20.00mL test solution was placed in 50mL colorimetric tube,
Add 5 mL of acetate buffer solution, 10 mL of saturated hydrogen sulphide water, dilute to the mark, shake, in the dark place 5min. On white background
Observed, it was the color can not be deeper than the standard colorimetric solution.
Preparation of standard color solution ratio. Pipette 2mL lead standard solution in 50mL colorimetric tube, add water to 20mL, add 5 mL of acetate buffer
Diluted solution, 10 mL saturated solution of hydrogen sulfide with water to the mark, shake, in the dark place 5min. Simultaneously with the sample.
A.8 Determination of Lead
A.8.1 graphite furnace atomic absorption spectrophotometry (Arbitration Act)
A.8.1.1 Reagents and materials
A.8.1.1.1 nitric acid solution. about 0.5mol/L;
Take 32mL of nitric acid was added to water, diluted to 1000mL.
A.8.1.1.2 Lead standard solution. 1mL solution containing lead (Pb) 100ng;
Pipette Pipette 1mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark with a solution of nitric acid
Degree, shake. After Pipette solution was diluted with 5mL 500mL volumetric flask, dilute nitric acid solution to the mark. The solution was formulated before use.
A.8.1.1.3 two water. in line with GB/T 6682-2008 requirements.
A.8.1.2 instruments and equipment
Are nitric acid solution (15) soaked overnight with water repeatedly washed with deionized water rinse. A.8.1.2.1 The glassware used.
A.8.1.2.2 atomic absorption spectrophotometer (with furnace and lead hollow cathode lamp).
A.8.1.3 analysis step
A.8.1.3.1 Preparation of test solution
Weigh about 0.2g sample accurate to 0.01g, a 50mL beaker was added nitric acid to dissolve the sample was transferred to a 25mL volumetric flask
The nitric acid solution was diluted to the mark.
Blank test solution prepared simultaneously. In addition to the blank test solution without the sample, the type and amount of addition of reagents and other operations with the Test Phase
with.
A.8.1.3.2 curve plotted
Pipette respectively lead standard solution 0.00mL, 5.00mL, 10.00mL, 20.00mL in four 50mL volumetric flask, add dilute nitric acid solution
Release to the mark. This series of concentration was 0 ng/mL, 10ng/mL, 20ng/mL, 40ng/mL. Each draw 10μL, injection stone
Mexican furnace, measured obtaining the absorbance, the concentration of lead as abscissa and ordinate corresponding absorbance, drawing working curve.
A.8.1.3.3 Determination
At a wavelength of 283.3nm at the instrument adjusted to the best working condition, respectively Pipette test solution and the blank test solution 10μL, injection graphite furnace,
Obtaining the measured absorbance, check the content to give the corresponding lead from the working curve.
A.8.1.4 Calculation Results
Lead content of lead (Pb) mass fraction w4 and its value in mg/kg according to formula (A.5) Calculated.
2510) (
ccw × - = (A.5)
Where.
Numerical test solution c1-- isolated from the working curve of lead content, expressed in nanograms per milliliter (ng/mL);
c0 - Numerical blank test solution is isolated from the working curve of lead content, expressed in nanograms per milliliter (ng/mL);
m - the value of the sample mass, in grams (g);
25-- test correctly predicted capacity volume in milliliters (mL).
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.8.2 Pyrrolidine dithiocarbamate (The APDC) Extraction
A.8.2.1 Reagents and materials
A.8.2.1.1 sulfuric acid.
A.8.2.1.2 hydrochloric acid.
A.8.2.1.3 nitrate.
A.8.2.1.4 chloroform.
A.8.2.1.5 sodium hydroxide solution. 250g/L;
Weigh 25g of sodium hydroxide in 200mL plastic beaker, dissolved in 100mL of water.
A.8.2.1.6 Pyrrolidine dithiocarbamate (The APDC) solution. 20g/L;
Dissolving 2g Pyrrolidine dithiocarbamate (The APDC) in 100mL of water. Filtered before use.
A.8.2.1.7 Lead standard solution. 1mL solution containing lead (Pb) 0.005mg;
Pipette pipette 5mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark with water, shake
uniform. The solution was formulated before use.
A.8.2.1.8 precision pH test paper. pH0.5 ~ 5.0.
A.8.2.1.9 two water. in line with GB/T 6682-2008 requirements.
A.8.2.2 instruments and equipment
Are nitric acid solution (15) soaked overnight with water repeatedly washed with deionized water rinse. A.8.2.2.1 The glassware used.
A.8.2.2.2 separating funnel. 250mL.
A.8.2.2.3 atomic absorption spectrophotometer (with lead hollow cathode lamp).
A.8.2.3 analysis step
A.8.2.3.1 Preparation of test solution
Weigh about 5g sample, accurate to 0.01g, placed in 150mL beaker, add 30mL water is added 1mL hydrochloric acid. Heat to boil a few minutes,
Cooled, diluted to 100mL, the solution was adjusted to pH 1.0 with sodium hydroxide solution to 1.5. The solution was transferred to a 250mL separatory funnel, with
Diluted with water to about 200mL. Add 2mL Pyrrolidine dithiocarbamate (The APDC) solution, and mixed. Extracted with chloroform twice
Added 20 mL, the extract was collected in 50mL beaker, steam bath and evaporated to dryness (this operation must be carried out in a fume hood), was added to the residue
3mL of nitric acid and continue to evaporate to near dryness. Nitric acid was added 0.5mL and 10mL water was heated until the solution volume of approximately 3mL ~ 5mL. Transferred to
10mL volumetric flask, dilute to the mark, shake.
Preparation A.8.2.3.2 blank test solution
Taking into 30mL water 150mL beaker was added 1mL of hydrochloric acid. Heat to boil a few minutes, cooled, diluted to 100mL. Hydroxide
The solution was adjusted to pH sodium 1.0 to 1.5. The following operation is the same in A.8.2.3.1 "This solution was transferred to a separatory funnel and transferred to a 250mL 10mL
Volumetric flask and diluted with water to the mark. "
A.8.2.3.3 Preparation of standard solution
Pipette 4.00mL lead standard solution was placed in 150mL beaker, add 30mL water is added 1mL hydrochloric acid. Heat to boil a few minutes, cooled,
Diluted to 100mL. The solution was adjusted to pH 1.0 with sodium hydroxide solution to 1.5. The following operation is the same in A.8.2.3.1 "This solution was transferred to 250mL
Transferred to a separatory funnel 10mL volumetric flask, diluted with water to the mark. "
A.8.2.3.4 Determination
A.8.2.3.4.1 instrument conditions. resonance line 283.3nm; slit 0.7nm; air - acetylene flame.
A.8.2.3.4.2 Determination. The test solution, standard solution to import atomic absorption spectrophotometer, zero blank test solution, absorption was measured
Absorbance value closing, the sample can not be higher than the standard solution absorbance.
A.9 pH measurement
A.9.1 Instruments and Equipment
pH meter. dividing the value 0.02.
A.9.2 Analysis step
Weigh 1.00g ± 0.01g sample was placed in 150mL beaker, add 100mL water dissolved carbon dioxide-free samples. Use has been proofread
pH meter.
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 0.1.
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