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GB 25558-2010: National food safety standards for food additives, tricalcium phosphate
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National food safety standards for food additives, tricalcium phosphate
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GB 25558-2010
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Basic data | Standard ID | GB 25558-2010 (GB25558-2010) | | Description (Translated English) | National food safety standards for food additives, tricalcium phosphate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 15,135 | | 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 calcium hydroxide (or calcium carbonate) and thermal phosphoric acid as raw food additive tricalcium phosphate or calcium chloride solution with trisodium phosphate for raw materials, food additive tricalcium phosphate. | GB 25558-2010: National food safety standards for food additives, tricalcium phosphate---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.
National food safety standards for food additives, tricalcium phosphate
National Food Safety Standard
Food additives tricalcium 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 tricalcium phosphate
1 Scope
This standard applies to calcium hydroxide (or carbonate) with thermal phosphoric acid as raw materials, food additives tricalcium phosphate or calcium chloride solution
Solution of trisodium phosphate for raw materials and food additives tricalcium 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.
Formula 3
Approximate components. 10CaO · 3P2O5 · H2O
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. Organization Status powder
4.2 Physical indicators. to comply with Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Tricalcium phosphate (Ca in terms), w /% 34.0 ~ 40.0 Appendix A A.4
Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.5
Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.6
Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.7
Fluorides (as F)/(mg/kg) ≤ 75 Appendix A A.8
Loss on ignition, w /% ≤ 10.0 A.9 in Appendix A
Clarity through test A.10 in Appendix A
Appendix A
(Normative)
Testing method
A.1 Warning
Reagents The standard test methods used for toxic or corrosive, be careful when operating! As should be immediately splashed on the skin
Rinsed with water, severe cases should be treated immediately. When using the virulent, should be strictly in accordance with the relevant provisions of the management, avoid inhalation or contact with the skin,
Necessary, should be carried out in a fume hood. For persons exposed parts of the wound can not touch. When possible operation, should be ventilated hood intake
Row.
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 nitrate.
A.3.1.2 hydrochloric acid solution. 14.
A.3.1.3 ammonium oxalate solution. 33 g/L.
A.3.1.4 ammonium molybdate solution. Weigh 2.5g of ammonium molybdate [(NH4) 6Mo7O24 · 4H2O], sulfuric acid 15mL dissolved, diluted with water to about 100mL.
Using the period of one week.
A.3.2 Analysis step
A.3.2.1 Identification of calcium ions
0.1g of sample was dissolved in 5mL 5mL hydrochloric acid solution and hot water, was added dropwise with stirring 1mL ammonium oxalate solution, it should be a white precipitate.
A.3.2.2 Identification of phosphate
The 0.1g sample was wetted with water, a solution of nitric acid to dissolve, a little heat, if necessary, a solution of ammonium molybdate solution, should produce a yellow precipitate.
A.4 Determination of tricalcium phosphate
A.4.1 disodium edetate direct titration (Arbitration Act)
A.4.1.1 Method summary
The sample was dissolved in hydrochloric acid, was added a solution of triethanolamine as a masking agent for masking the influence of interference ions, B was added dropwise under acidic conditions
Diamine tetra acetic acid disodium standard titration solution near the end, the test solution with sodium hydroxide to adjust the pH value to hydroxy naphthol blue indicator color
The pH range, continue to titrate the remaining calcium.
A.4.1.2 Reagents and materials
A.4.1.2.1 triethanolamine.
A.4.1.2.2 hydrochloric acid solution. 11.
A.4.1.2.3 sodium hydroxide solution. 450 g/L.
A.4.1.2.4 disodium EDTA standard titration solution. c (EDTA) = 0.05 mol/L.
A.4.1.2.5 hydroxy naphthol blue indicator;
Weigh 10 g at 105 ℃ ± 2 ℃ drying 2 h at sodium chloride, into a mortar, was added 0.1 g hydroxy naphthol blue indicator, fine,
Mix well. Placed in the weighing bottle, stored in a desiccator. Use period is two months.
A.4.1.3 instruments and equipment
Magnetic stirrer.
A.4.1.4 analysis step
Weigh 0.15 g samples, accurate to 0.000 2 g, equipped with a magnetic stirrer was placed in a 250 mL beaker, add a little water to make a sample Run
Wet, 5 mL of hydrochloric acid was dissolved, when necessary, to be slowly heated carefully added 125 mL of water, while stirring continuously sequentially 0.5 mL of
Triethanolamine, 0.3 g hydroxy naphthol blue indicator, dropping buret at normal speed disodium edetate standard titration solution of about 23mL ~
27 mL (amount should be equivalent to 90% to 95% calcium content), sodium hydroxide solution was added dropwise to the original red to blue, 71/92
To blue to purple, then excess 0.5 mL, pH then the solution should be between 12.3 to 12.5. Continue to use the standard disodium edetate
Titration titration solution until the solution appears clear blue, holding 60 s unchanged. At the same time a blank test.
In addition to the blank test without the sample, the addition of reagents and other operations of the kind and amount (other than the standard titration solution) with the same Test.
A.4.1.5 Calculation Results
Tricalcium phosphate, calcium (Ca) mass fraction w1 and its value is expressed in%, according to formula (A.1) calculated as follows. []
1000) 0
1 × - = m
cMVV
((A.1)
Where.
Numerical V-- titration solution consumed disodium EDTA standard titration solution volume in milliliters (mL);
Numerical V0-- blank test consumed disodium EDTA standard titration solution volume in milliliters (mL);
Accurate c-- disodium edetate standard titration solution concentration value in units of moles per liter (mol/L);
Numerical m-- sample mass, expressed in grams (g);
Numerical M-- calcium (Ca) molar mass of the units of grams per mole (g/mol) (M = 40.078).
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 zinc sulfate back titration
A.4.2.1 Method summary
In the test solution, adding an excess of disodium EDTA standard titration solution, and calcium ion complexation to the mixture as a means KB
Shows agents, zinc standard titration solution titrate excess of disodium edetate standard titration solution.
A.4.2.2 Reagents and materials
A.4.2.2.1 hydrochloric acid solution. 1 + 1.
A.4.2.2.2 ammonia - ammonium chloride buffer solution (A). pH≈10.
A.4.2.2.3 disodium ethylene diammonium standard titration solution. c (EDTA) = 0.05 mol/L.
A.4.2.2.4 acid chrome blue K- naphthol green B mixed indicator solution (KB indicator solution).
A.4.2.2.5 zinc sulfate standard titration solution. c (ZnSO4 · 7H2O) = 0.05 mol/L;
Preparation. Weigh 15 g zinc sulfate, dissolved in water, diluted with water to 1000 mL, shake.
Calibration. Pipette 25.00 mL zinc sulfate standard titration solution prepared, placed in a conical flask, add 10 mL of ammonia - ammonium chloride buffer solution and
75 mL of water, add about 0.02 g chrome black T indicator, with 0.05 mol/B diammonium disodium titration standard solution titration solution from purple to L
Color to pure blue, and held 30 s does not fade, is the end. At the same time a blank test.
In addition to the blank test without the sample, the addition of reagents and other operations of the kind and amount (other than the standard titration solution) with the same Test.
Zinc sulfate standard titration solution concentration c according to equation (A.2) Calculated.
c =
cVV 101) (- (A.2)
Where.
Numerical diammonium acetate disodium titration V1-- standard titration solution consumed volume in milliliters (mL);
Numerical V0-- blank test consumption of diammonium acetate disodium standard titration solution volume in milliliters (mL);
Accurate c1-- disodium ethylene diammonium standard titration solution concentration value in units of moles per liter (mol/L);
Numerical volume V-- Pipette zinc sulfate standard titration solution, in milliliters (mL).
A.4.2.3 analysis step
Weigh about 0.5 g samples, accurate to 0.000 2 g, placed in 100 mL beaker with a small amount of water wet, add 5 mL of hydrochloric acid solution so that the whole sample
Ministry of dissolution, if necessary, dried and filtered. All transferred to 250 mL volumetric flask, dilute to the mark, shake.
Pipette 25.00 mL above test solution, placed in 500 mL conical flask, and then moved to 25.00 mL of disodium ethylene diammonium standard titration solution
Solution, add 50 mL of water, 10 mL of ammonia - ammonium chloride buffer solution (A) shake for 5 min. Add about 2 to 3 drops KB drops indicator solution with zinc sulfate
Standard Solution titration until the solution changed from blue to blue-violet, purple and held within 30 s does not fade, is the end. At the same time a blank test.
In addition to the blank test without the sample, the addition of reagents and other operations of the kind and amount (other than the standard titration solution) with the same Test.
A.4.2.4 Calculation Results
Tricalcium phosphate, calcium (Ca) mass fraction w1 and its value is expressed in%, according to formula (A.3) calculated as follows. []
1000) 10
1 ××
- =
cMVV
((A.3)
Where.
Numerical zinc sulfate standard titration V0-- blank test solution consumed volume in milliliters (mL);
Numerical zinc sulfate standard titration solution consumed V1-- titration solution volume in milliliters (mL);
Accurate c-- zinc sulfate standard titration solution concentration value in units of moles per liter (mol/L);
m-- sample mass value in grams (g);
Numerical M-- calcium (Ca) molar mass of the units of grams per mole (g/mol) (M = 40.078).
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 Heavy Metals
A.5.1 Reagents and materials
A.5.1.1 hydrochloric acid solution. 1 + 4.
A.5.1.2 hydrogen sulphide saturated aqueous solution .( The preparation before use).
A.5.1.3 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. The solution is using now.
A.5.1.4 other agents with GB/T 5009.74-2003 in Chapter 3.
A.5.2 Instruments and Equipment
With GB/T 5009.74-2003 Chapter 4.
A.5.3 Analysis step
After weighing 2.00 g ± 0.01 g sample was placed in a 50 mL beaker, add 5 mL hydrochloric acid solution and 10 mL of water, dissolved by heating, cooling
Dropping ammonia to white precipitate appeared with filter paper and the filtrate was placed in 100 mL volumetric flask, dilute to the mark, shake. Pipette
25.00 mL above test solution was placed in 50 mL colorimetric tube, add 5 mL of acetate buffer solution, mix, add 5 drops of saturated hydrogen sulphide water,
And diluted with water to the mark, mixing, placing in the dark for 5 min. The color was not be deeper than the standard colorimetric solution.
Color than the standard preparation solution. Pipette 0.50 mL of lead standard solution was placed in 50 mL colorimetric tube, add 25 mL of water, from the "plus 5 mL
Acetate buffer solution "began to operate simultaneously with the test solution the same treatment.
A.6 Determination of Lead
A.6.1 dithizone colorimetry (Arbitration Act)
A.6.1.1 Method summary
With GB/T 5009.75─2003 Chapter 2.
A.6.1.2 Reagents and materials
With GB/T 5009.75─2003 Chapter 3.
A.6.1.3 instruments and equipment
With GB/T 5009.75─2003 Chapter 4.
A.6.1.4 analysis step
Weigh 5.00 g ± 0.01 g sample was placed in 100 mL beaker, add water wet, add appropriate amount of hydrochloric acid to dissolve, placed in a separatory funnel.
Pipette 1.00 mL of lead standard solution, placed in a separatory funnel as standard colorimetric solution, the following according to GB/T 5009.75─2003 6
Chapter predetermined measurement.
A.6.2 Atomic absorption spectrophotometry
A.6.2.1 Reagents and materials
A.6.2.1.1 hydrochloric acid.
A.6.2.1.2 chloroform.
A.6.2.1.3 nitrate.
A.6.2.1.4 sodium hydroxide solution. 250 g/L.
A.6.2.1.5 Pyrrolidine dithiocarbamate (The APDC) solution. 2%;
Weigh 2 g Pyrrolidine dithiocarbamate (The APDC) was dissolved in 100 mL of water. If insoluble material filtered before use.
A.6.2.1.6 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. The solution is using now.
A.6.2.1.7 precision pH test paper. pH 0.5 ~ 5.0.
A.6.2.1.8 two Water. comply with GB/T 6682-2008 of.
A.6.2.2 instruments and equipment
A.6.2.2.1 separating funnel. 250 mL.
A.6.2.2.2 constant temperature water bath.
A.6.2.2.3 atomic absorption spectrophotometer.
A.6.2.3 analysis step
A.6.2.3.1 Determination of lead standard preparation and assay solutions
Accurate Pipette 2.00 mL of lead standard solution, placed in a 150 mL beaker, add 30 mL of water, 10 mL of hydrochloric acid, (surface covered dish) plus
Heat to boiling and boil 5 min. Cooling, the solution was adjusted with a sodium hydroxide solution of pH 1.0 to 1.5 (pH paper with a precision test). The solution
It was transferred to a separatory funnel, diluted with water to approximately 200 mL. Added 2 mL of pyrrolidine dithio carbamate (APDC) solution, shake.
Chloroform extracted twice, each added 20 mL, the extract (ie, organic phase) was collected in 50 mL beaker (in a fume hood)
Heated water bath evaporated to dryness. 3 mL of nitric acid was added to the residue and heated nearly dry. Was added 0.5 mL of nitric acid and 10 mL of water and heated to left
More than liquid volume was 3 mL ~ 5 mL, transferred to 10 mL volumetric flask, dilute to the mark with water. Selection of air - acetylene flame at 283.3 nm
Wavelength, zero water, measuring the absorbance of the solution.
Preparation and determination of sample measurement solutions A.6.2.3.2
Weigh 10.0 g ± 0.1 g sample is placed in a 150 mL beaker, add 30 mL of water, 10 mL of hydrochloric acid (surface covered dish) plus
Heat to dissolve the sample, and boiled 5 min. Then press A.6.2.3.1 from the "cooling with sodium hydroxide solution to adjust the pH," begins operating,
Measuring the corresponding absorbance.
A.6.2.4 results found
Determination of the sample solution is not greater than the absorbance of lead standard measuring the absorbance of the solution.
A.7 Determination of Arsenic
A.7.1 Reagents and materials
A.7.1.1 hydrochloric acid solution. 1 + 1.
A.7.1.2 arsenic standard solution. 1 mL solution containing arsenic (As) 0.001mg;
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.7.1.3 other agents with GB/T 5009.76-2003 of Chapter 9.
A.7.2 Instruments and Equipment
With GB/T 5009.76-2003 Chapter 10.
A.7.3 Analysis step
Weigh 0.50 g ± 0.01 g sample was placed in a given arsenic bottle, add a small amount of water wet, add 5 mL of hydrochloric acid solution to dissolve the sample.
Limits formulated solution. Pipette 1.50 mL of arsenic standard solution, given arsenic placed in the bottle, the following according to GB/T 5009.76-2003 first
The provisions of Chapter 11 was measured.
A.8 Determination of fluoride
A.8.1 Reagents and materials
A.8.1.1 hydrochloric acid solution. 14.
A.8.1.2 total ionic strength buffer. sodium acetate solution was mixed with an equal amount of sodium citrate solution, and the solution using now.
A.8.1.3 sodium acetate solution. c (CH3COONa · 3H2O) = 3 mol/L;
Weigh 204 g of sodium acetate dissolved in about 300 mL of water, cooled, 1 mol/L acetic acid adjusted pH≈7.0, all transferred to 500 mL
Volumetric flask and diluted with water to the mark.
A.8.1.4 sodium citrate solution. c (Na3C6H5O7 · 2H2O) = 0.75 mol/L;
Weigh 110 g of sodium citrate, dissolved in about 300 mL of water, heightening acid 14 mL, all transferred to 500 mL volumetric flask, dilute with water
Release to the mark.
A.8.1.5 fluoride standard solution. 1mL 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. The solution now with the existing, stored in a polyethylene bottle.
A.8.2 Instruments and Equipment
A.8.2.1 fluorine electrode.
A.8.2.2 calomel electrode.
A.8.2.3 potentiometer.
A.8.2.4 magnetic stirrer.
A.8.3 Analysis step
A.8.3.1 preparation of standard working solution
Pipette fluoride standard solution 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL were placed in five 50 mL volumetric flask
, Each of the hydrochloric acid solution was added 4 mL, add 25 mL of total ionic strength buffer, diluted with water to the mark.
A.8.3.2 Preparation of test solution
Weigh a sample of about 1 g, accurate to 0.01 g, was added 4 mL of hydrochloric acid solution, 25 mL of total ionic strength buffer, dissolved into 100 mL
Volumetric flask, dilute to the mark, shake.
A.8.3.3 Determination
The fluoride ion selective electrode and calomel electrode and the potentiometer negative and a positive terminal coupled to the electrode insert filled with water 50 mL polyethylene plastic beaker,
Preheat the instrument, on a magnetic stirrer with constant stirring, to read the value of the equilibrium potential, the replacement of water soaking the electrode to electrode specified in the instructions
After the potential value to the standard working solution and the potential of the sample solution was measured.
Equilibrium potential fluoro standard working solution were measured from low to high concentrations. Electrode potentials as ordinate, the fluorine ion concentration (mg/mL)
As abscissa, the curve on semi-logarithmic graph paper.
The same method the equilibrium potential of the sample solution, the concentration of fluoride ions in the sample (mg/mL), isolated from the working curve.
A.8.4 Calculation Results
Fluoride content of fluorine (F) mass fraction w2 and its value in mg/kg according to formula (A.4) Calculated.
- ×
× =
cw (A.4)
Where.
C-- value from the working curve Richard fluoride ion concentration, in milligrams per milliliter (mg/mL);
m - value the quality of the sample, 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 10 mg/kg.
A.9 Determination of loss on ignition
A.9.1 Instruments and Equipment
A.9.1.1 porcelain crucible. 30 mL.
A.9.1.2 furnace temperature. The temperature can be controlled at 800 ℃ ± 50 ℃.
A.9.2 Analysis step
Was used at 800 ℃ ± 50 ℃ condition 30 min burning porcelain crucible, weigh about 2 g samples, accurate to 0.0002 g, placed in a high temperature furnace
Within, at 800 ℃ ± 50 ℃ burning conditions 30 min, remove the cooling to room temperature, placed in a desiccator, and weigh.
A.9.3 Calculation Results
LOI mass fraction w3 and its value is expressed in%, according to formula (A.5) Calculated.
0213 × - = m
mmw (A.5)
Where.
m1-- before burning the sample values and quality porcelain crucible in units of grams (g);
Numerical m2-- residue after burning and porcelain 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 0.2%.
A.10 Determination of Clarity
A.10.1 reagents and materials
A.10.1.1 hydrochloric acid solution; 1 + 1.
A.10.1.2 nitrate solution. 1 + 2.
A.10.1.3 silver nitrate solution. 20 g/L.
A.10.1.4 chloride standard solution. 1 mL solution of chlorine (Cl) 0.010 mg;
Pipette 1.00 mL of chloride 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. The solution is using now.
A.10.2 instruments and equipment
Constant temperature water bath.
A.10.3 Analysis steps
Weigh 2.00 g ± 0.01 g sample was placed in a 50 mL beaker, add 18 mL of water and 8 mL of hydrochloric acid solution, heated in a boiling water bath for 5 min
Dissolved. All transfer After cooling to 50 mL colorimetric tube, diluted with water to the mark. Turbidity is not greater than the standard sample solution turbidity was
The turbidity of the solution through the test.
Turbid than the standard preparation solution. Pipette 6.00 mL chloride standard solution, placed in 50 mL colorimetric tube, add 20 mL water, 1 mL
Dilute nitric acid solution, 1 mL of silver nitrate solution with water to the mark. Placed 15 min in the dark.
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