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GB 25572-2010: The national food safety standards of food additives calcium hydroxide
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The national food safety standards of food additives calcium hydroxide
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Basic data | Standard ID | GB 25572-2010 (GB25572-2010) | | Description (Translated English) | The national food safety standards of food additives calcium hydroxide | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 14,172 | | 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 limestone or oyster shells containing limestone and other raw materials by calcination, digestion of food additives made ??of calcium hydroxide. | GB 25572-2010: The national food safety standards of food additives calcium hydroxide---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.
The national food safety standards of food additives calcium hydroxide
National Food Safety Standard
Food additives calcium hydroxide
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 calcium hydroxide
1 Scope
This standard applies to limestone containing limestone or oyster shells as raw materials calcined, from the digestion of food additives calcium hydroxide.
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
Ca (OH) 2
3.2 relative molecular mass
74.09 (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 50mL beaker, observe the color in natural light
And texture. Organization Status powder
4.2 Physical indicators. to comply with Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Calcium hydroxide [Ca (OH) 2], w /% 95.0 ~ 100.5 Appendix A A.4
Carbonate by test A.5 in Appendix A
Magnesium and alkali metal, w /% ≤ 2.0 A.6 in Appendix A
Acid insoluble, w /% ≤ 0.1 Appendix A A.7
Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.8
Fluorides (as F)/(mg/kg) ≤ 50 Appendix A A.9
Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.10
TABLE 2 (cont.)
Item Index Test Method
Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.11
Loss on drying, w /% ≤ 1.0 Appendix A A.12
Sieve residue (0.045mm), w /% ≤ 0.4 Appendix A A.13
Appendix A
(Normative)
Testing method
A.1 Warning
Reagents The standard test methods used in corrosive, be careful when operating! As splashed on the skin should immediately wash with water,
In severe cases should be treated immediately. When using the virulent, should be strictly managed in accordance with relevant regulations; should be used to avoid inhalation or contact with the skin, if necessary
It should be carried out in a fume hood. Exposed parts of the wound can not touch people.
A.2 General Provisions
The standard test methods used in the reagents and water in the absence of other specified requirements, refer to analytically pure reagents and GB/T 6682-2008 specified
Tertiary water. Test with the standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according
HG/T 3696.1, HG/T 3696.2, the provisions prepared HG/T 3696.3 of.
A.3 Identification Test
A.3.1 Reagents and materials
A.3.1.1 acetic acid solution. 11.
A.3.1.2 ammonium oxalate solution. 40g/L.
Weigh 4g ammonium oxalate (C2H8N2O4 • H2O) dissolved in 100mL of water.
A.3.1.3 red litmus paper.
A.3.2 Analysis step
A.3.2.1 Identification of hydroxide ions
Weigh about 5g sample was added 20mL of water are mixed, forming a thick paste sample, the upper supernatant make a thick paste of red litmus paper blue.
A.3.2.2 Identification of calcium ions
1g sample with 20mL of water are mixed, add enough acetic acid to dissolve the sample, add ammonium oxalate solution, to form insoluble oxalate precipitation. this
The precipitate is insoluble in acetic acid and dissolved in hydrochloric acid.
A.4 Determination of calcium hydroxide
A.4.1 Method summary
Take appropriate test solution, sucrose masking interference carbonate phenolphthalein as indicator, titrated with standard hydrochloric acid solution was titrated to colorless.
A.4.2 Reagents and materials
A.4.2.1 hydrochloric acid standard titration solution. c (HCl) = 0.5mol/L.
A.4.2.2 sucrose solution. 300g/L.
It weighs 300g sugar, dissolved in 1000mL water. Add 1 drop of phenolphthalein indicator solution, prior to use was added dropwise a solution of sodium hydroxide (4g/L) until the solution just
It was slightly pink.
A.4.2.3 phenolphthalein indicator solution. 10g/L.
A.4.3 Instruments and Equipment
Electromagnetic stirrer.
A.4.4 Analysis step
Weigh approximately 0.5g of the sample to the nearest 0.000 2g, placed in 250mL conical flask, add 50mL water, shaking it and mix. Join
50mL sucrose solution using a magnetic stirrer for 15min, add 2 drops to 3 drops of phenolphthalein indicator solution, titration with standard hydrochloric acid solution was titrated to
Just test solution becomes colorless, and keep the 30s does not return color is the end.
Meanwhile blank test, in addition to omission of sample addition, the same amount of reagent was added and the other test solution (hydrochloric acid standard titration solution except),
And the sample at the same time the same treatment.
A.4.5 Calculation Results
Calcium hydroxide content of calcium hydroxide [Ca (OH) 2] mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated.
1000) (0
1 × - = m
MVVc
w (A.1)
Where.
Accurate c-- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L);
Hydrochloric acid standard titration solution volume V-- test solution consumed value in milliliters (mL);
V0-- blank test solution consumption hydrochloric acid standard titration solution volume value in milliliters (mL);
Quality m-- sample value in units of grams (g);
M-- calcium hydroxide [1/2Ca (OH) 2] molar mass values, expressed in gram per mole (g/mol) (M = 37.05).
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.5 Determination of carbonate
A.5.1 Reagents and materials
Hydrochloric acid solution. 13.
A.5.2 Analysis step
Weigh about 2g samples, accurate to 0.01g, was added 50mL of water, mix, add 40mL hydrochloric acid solution, the dissolution process should be just fine
Bubble generation.
A.6 Determination of magnesium and alkali metals
A.6.1 Reagents and materials
A.6.1.1 sulfuric acid.
A.6.1.2 hydrochloric acid solution. 13.
A.6.1.3 ammonia solution. 11.
A.6.1.4 oxalic acid. 63g/L.
Weigh 6.3g of oxalic acid (H2C2O4 • 2H2O) was dissolved in 100mL of water.
A.6.1.5 methyl red indicator solution. 1g/L.
A.6.2 Instruments and Equipment
High-temperature furnace. temperature can be controlled at 800 ℃ ± 25 ℃.
A.6.3 Analysis step
Weigh about 0.5g sample to the nearest 0.000 2g, was added 10mL of water and hydrochloric acid solution 6mL make sample dissolution boil 1min. Rapid increase
Oxalic acid solution into 40mL, with vigorous stirring. Add 2 drops of methyl red indicator solution, dropping ammonia solution to yellow solution, this mixture was cooled
Was transferred to 100mL volumetric flask, dilute to the mark, shake. 4h or stand overnight. Medium speed dry filter paper, discard the initial liquid 10mL.
Pipette pipette 50mL filtrate was previously at 800 ℃ ± 25 ℃ calcined to constant mass in a porcelain crucible, was added 0.5mL of sulfuric acid, steam bath
Send to nearly dry (or on the electric low temperature evaporation to near dryness). On a hotplate and then carefully evaporated to dryness. Continue heating the ammonium salt completely decomposed and evaporated.
Placed in a high temperature furnace, burning at 800 ℃ ± 25 ℃ to constant mass.
A.6.4 Calculation Results
Magnesium and alkali metal content of the mass fraction w2 and its value is expressed in%, according to formula (A.2) Calculated.
) 01050 (
twenty one
2 ××
- =
mmw (A.2)
Where.
Numerical m1-- porcelain crucible and residue mass in grams (g);
Numerical m2-- 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.7 Determination of acid-insoluble matter
A.7.1 Reagents and materials
A.7.1.1 hydrochloric acid solution. 13.
A.7.1.2 silver nitrate solution. 17g/L.
A.7.2 Instruments and Equipment
A.7.3.1 sand core glass crucible. pore size 5μm ~ 15μm.
A.7.3.2 electric oven. temperature can be controlled at 105 ℃ ± 2 ℃.
A.7.3 Analysis step
Weigh about 4g sample, accurate to 0.0002g, add a small amount of water wetting, 60mL hydrochloric acid solution was added to dissolve the sample, bring to the boil. With pre
First at 105 ℃ ± 2 ℃ drying to constant quality glass sand core crucible hot filtration, the filtrate was washed with hot water until no chloride ions (silver nitrate solution
test). Placed in the electric oven at 105 ℃ drying to constant mass ± 2 ℃. Cool to room temperature in a desiccator, and weigh.
A.7.4 Calculation Results
Acid insoluble mass fraction w3 and its value is expressed in%, according to formula (A.3) Calculated.
0213 × - = m
mm
w (A.3)
Where.
Numerical m1-- glass sand core crucible and residue mass in grams (g);
Numerical m2-- glass sand core crucible mass 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 0.03%.
A.8 Determination of Arsenic
A.8.1 Reagents and materials
A.8.1.1 hydrochloric acid solution. 13.
A.8.1.2 Other agents with GB/T 5009.76-2003 of Chapter 9.
A.8.2 Instruments and Equipment
With GB/T 5009.76-2003 Chapter 10.
A.8.3 Analysis step
Weigh 0.50g ± 0.01g sample was placed in a conical flask. Hydrochloric acid solution was added 10mL (A.8.1.1) to dissolve the sample. Hydrochloric acid was added 4mL to
Operating with GB/T 5009.76-2003 in Chapter 11, "add water to 30mL, plus 5mL15% potassium iodide solution can not be deeper than the limit of arsenic
Standard Gutzeit. "
Limits formulated solution. Pipette 1.00mL arsenic standard solution (1mL solution arsenic 1.00μg), the following actions with GB/T 5009.76
-2003 In Chapter 11, "plus 5mL hydrochloric acid removed Gutzeit compare."
A.9 Determination of fluoride
A.9.1 Reagents and materials
A.9.1.1 hydrochloric acid solution. 111.
A.9.1.2 hydrochloric acid solution. 13.
A.9.1.3 sodium acetate solution. 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.9.1.4 sodium citrate solution. 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.9.1.5 total ionic strength buffer.
Sodium acetate solution was mixed with an equal amount of sodium citrate solution, prior to use the preparation.
A.9.1.6 fluoride standard solution. 1mL solution of fluorine (F) 0.010mg.
Pipette 1.00mL fluoride standard solution according to HG/T 3696.2 prepared, placed in 100mL flask, diluted with water to the mark.
The solution was formulated before use.
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 magnetic stirrer.
A.9.2.4 Potentiometer. Indexing is 0.02.
A.9.3 Analysis step
Prepare A.9.3.1 Instrument
The fluoride ion selective electrode (by manual activation) and a saturated calomel electrode and the negative terminal of the measuring instrument connected to the positive terminal of the electrode insert containing
After 50mL plastic cup of water, electromagnetic stirring (polyethylene rotor), read the value of the equilibrium potential, the replacement of 2 to 3 times the water, to be potential
After the value of the equilibrium potential measurement can be carried out.
A.9.3.2 Determination
Weigh about 1g sample to the nearest 0.01g. A 50mL beaker, add water wet, add 15mL hydrochloric acid solution (A.9.1.2) make
The sample is dissolved. Boil 1min, after cooling, transferred to a 50mL volumetric flask, add 25mL total ionic strength buffer, add water to the mark.
Poured into a plastic beaker 50mL measuring electrode potential.
A.9.3.3 draw the curve
Pipette respectively 1.00mL, 2.00mL, 4.00mL, 5.00mL, 6.00mL fluoride standard solution (equivalent to a fluorine-containing 0.010mg, 0.020mg,
0.040mg, 0.050mg, 0.060mg) in five 50mL volumetric flask, were added to each flask 25mL total ionic strength buffer, 10mL
Hydrochloric acid solution (A.9.1.1), diluted with water to the mark. Poured into a plastic beaker 50mL measuring 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
Quality value on the curve Richard fluorine.
A.9.4 Calculation Results
Fluoride content of fluorine (F) mass fraction w4 and its value in mg/kg according to formula (A.4) Calculated.
4 m
mw = (A.4)
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 more than 5 mg/kg.
A.10 Determination of Lead
A.10.1 graphite furnace atomic absorption spectrophotometry (Arbitration Act)
A.10.1.2 reagents and materials
A.10.1.2.1 nitrate.
A.10.1.2.2 nitric acid solution. 0.5mol/L.
The nitric acid was added 32mL of water, diluted to 1000mL.
A.10.1.2.3 ammonium dihydrogen phosphate solution. 20g/L.
Weigh 2.0g of ammonium dihydrogen phosphate, dissolved in water and diluted to 100mL.
A.10.1.2.4 lead standard solution. 1mL solution containing lead (Pb) 100ng.
Pipette 1.00mL lead standard solution according to HG/T 3696.2 formulated into 100mL volumetric flask, dilute nitric acid solution to the mark.
Then pipette take 5mL diluted solution in 500mL flask, diluted nitric acid solution to the mark. The solution before use with
system.
A.10.1.2.5 two water. in line with GB/T 6682-2008 requirements.
A.10.1.3 instruments and equipment
Are nitric acid solution (15) soaked overnight with water repeatedly washed with deionized water rinse. A.10.1.3.1 the glassware used.
A.10.1.3.2 atomic absorption spectrophotometer (with furnace and lead hollow cathode lamp).
A.10.1.4 analysis step
A.10.1.4.1 prepared test solution and the blank test solution
Weigh about 0.5g sample accurate to 0.01g, a 50mL beaker with water wetting, slowly dropped to about 1.5mL nitric acid, low temperature increase
Heat, until the sample is completely dissolved, heating steam until nearly dry, remove the cooled to room temperature, add 2 drops of nitric acid supplement, transferred to a 25mL volumetric flask
Diluted with water to the mark.
At the same time the preparation blank test solution, sample solution without addition, other types of addition of the reagents and the same number with the test solution, and at the same time
operating.
A.10.1.4.2 curve plotted
Pipette lead standard solution 0.00mL, 5.00mL, 10.00mL, 20.00mL, 30.00mL, 40.00mL to six 50mL capacity
Flask, dilute nitric acid solution to the mark, shake, this series of concentration was 0 ng/mL, 10ng/mL, 20ng/mL, 40ng/mL,
60ng/mL, 80ng/mL. Each draw 10μL, injection graphite furnace, measured obtaining the absorbance, the concentration of lead as abscissa and the corresponding absorbance
Ordinate drawing working curve.
A.10.1.4.3 Determination
At a wavelength of 283.3nm at the instrument adjusted to the best working condition, respectively draw test solution and blank solution 10μL, injection graphite furnace, measured
Absorbance, from the work of Richard curve corresponding concentrations of lead.
Use A.10.1.4.4 matrix modifier
If the interference, then inject the right amount of matrix modifier ammonium dihydrogen phosphate solution, typically 5μL or the same amount of the sample to eliminate interference. Draw Lead Standard
When the measurement sample was also added to the standard curve when the same amount of matrix modifier ammonium dihydrogen phosphate solution.
A.10.1.5 result of the calculation
Lead content of lead (Pb) mass fraction w5 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.10.2 dithizone spectrophotometry
A.10.2.1 reagents and materials
A.10.2.1.1 hydrochloric acid solution. 13.
A.10.2.1.2 other reagents with GB/T 5009.75-2003 in Chapter 3.
A.10.2.2 instruments and equipment
With GB/T 5009.75-2003 in Chapter 4.
A.10.2.3 analysis step
Weigh about 1g sample accurate to 0.01g, a 50mL beaker. After wetting with water, hydrochloric acid solution was added 15mL (A.10.2.1.1)
To dissolve the sample, transferred to a separatory funnel 125mL, 1% nitric acid solution was added to 20mL.
Make a blank test at the same time, but without addition of the sample, the other to join the same amount of reagent and test solution, and the sample simultaneously with the same treatment.
Following the same GB/T 5009.75-2003 6.2 "lessons lead standard solution drawing working curve."
A.10.2.4 result of the calculation
Lead content of lead (Pb) mass fraction w6 and its value in mg/kg according to formula (A.6) Calculated.
1000) (21
6 m
mmw - = (A.6)
Where.
m1 - the quality of the test solution to detect values of lead from the working curve, in micrograms (μg);
m2 - Numerical isolated blank test solution quality lead from the working curve, in micrograms (μg);
m - the value of the sample mass, in grams (g).
Take the arithmetic mean of the parallel determination results of the measurement results, the absolute value of two parallel determination results is not more than 1 mg/kg.
A.11 Determination of Heavy Metals (as Pb) of
A.11.1 reagents and materials
A.11.1.1 hydrochloric acid solution. 11.
A.11.1.2 hydrochloric acid solution. 13.
A.11.1.3 ammonia solution. 23.
A.11.1.4 acetate buffer solution. pH = 3.5.
Weigh 25.0 g ammonium acetate, add 25 mL of water is dissolved, add 45 mL of hydrochloric acid solution (A.11.1.1), then adjust the hydrochloric acid solution or aqueous ammonia solution
pH to 3.5, dilute to 100 mL.
A.11.1.5 sodium sulfide solution;
Weigh 5 g of sodium sulfide, add water to dissolve 10mL, 30mL glycerol added, mix, cover and sealed from light. Within three months after preparation
effective.
A.11.1.6 lead standard solution. 1mL solution containing lead (Pb) 0.01mg.
Pipette 1.00mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL flask, diluted with water to the mark. That
Solution preparation before use.
A.11.1.7 phenolphthalein indicator solution. 10g/L.
A.11.2 instruments and equipment
Colorimetric tube. 50mL.
A.11.3 Analysis steps
Weigh 2.00g ± 0.01g sample was placed in an evaporating dish, add water wet, hydrochloric acid solution was added 30mL (A.11.1.2) to dissolve the sample,
Steam bath to dry, add water to dissolve 20mL, filtered in colorimetric tube. Add 1 drop of phenolphthalein indicator solution, the solution was adjusted with ammonia Lawrence was slightly pink,
Add 5 mL of acetate buffer solution, dilute to the mark, add 1 drop of sodium sulfide solution, shake, in the dark place 5 min. White background
Observation was the color can not be deeper than the standard colorimetric solution.
Preparation of standard color solution ratio. Pipette 2.00mL lead standard solution for colorimetric tube, add water to 20mL, add 5 mL of acetate buffer solution,
Diluted with water to the mark, add 1 drop of sodium sulfide solution, shake, in the dark place 5 min. And sample simultaneously.
A.12 Determination of loss on drying
A.12.1 instruments and equipment
A.12.1.1 weighing bottle. Φ40 × 25mm.
A.12.1.2 electric oven. temperature can be controlled at 105 ℃ ± 2 ℃.
A.12.2 Analysis steps
Weigh about 2g samples, accurate to 0.0002g, placed beforehand at 105 ℃ ± 2 ℃ dried to constant mass weighing bottle and placed in an electric constant
Oven temperature at 105 ℃ ± 2 ℃ drying 1h... After cooling to room temperature in a desiccator, and weigh.
A.12.3 Calculation Results
Loss on drying mass fraction w7 and its value is expressed in%, according to formula (A.7) calculated as follows.
017 × - = m
mmw (A.7)
Where.
Numerical ago m-- dried sample mass, expressed in grams (g);
m1 - dried sample mass value in grams (g);
Take the arithmetic mean of the parallel determination results of the measurement results, the absolute value of two parallel determination results is not more than 0.03%.
A.13 Determination of sieve residue
A.13.1 instruments and equipment
A.13.1.1 Test sieves. R20/3 series, Ф200 × 50-0.045/0.032 GB/T 6003.1 -1997.
A.13.1.2 soft brush.
A.13.2 Analysis steps
It weighs about 10g sample to the nearest 0.01g. Moved within the test sieve with a soft brush lightly sample the powder through, finally, in a sieve under
Mat black paper, lightly sieve until the sample pad black paper no trace. The sieve residue is transferred to the surface of the dish known mass weighed to the nearest
0.0002g.
A.13.3 Calculation Results
Sieve residue mass fraction w8 and its value is expressed in%, according to formula (A.8) Calculated.
018 × = m
mw (A.8)
Numerical quality m1-- sieve residue in grams (g);
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 more than 0.04%.
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