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GB 25583-2010: The national food safety standards of food additives sodium aluminosilicate
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The national food safety standards of food additives sodium aluminosilicate
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Basic data | Standard ID | GB 25583-2010 (GB25583-2010) | | Description (Translated English) | The national food safety standards of food additives sodium aluminosilicate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Classification of International Standard | 67.220 | | Word Count Estimation | 12,171 | | 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 water glass prepared food additive sodium aluminosilicate. | GB 25583-2010: The national food safety standards of food additives sodium aluminosilicate---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 sodium aluminosilicate
National Food Safety Standard
Food additive sodium aluminosilicate
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 sodium aluminosilicate
1 Scope
This standard applies to food additive sodium aluminosilicate Preparation of water glass.
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 molar ratio of components
The molar ratio (molar ratio) Na2O/Al2O3/SiO2 is approximately 1. 1. 13.
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 and texture in natural light
status. Organization amorphous state fine powder or beads
4.2 Physical indicators. to comply with Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Silicon dioxide (SiO2), w /% 66.0 ~ 76.0 Appendix A A.4
Aluminum oxide (Al2O3), w /% 9.0 ~ 13.0 A.5 Appendix A
Sodium oxide (Na2O), w /% 4.0 ~ 7.0 A.6 in Appendix A
Lead (Pb)/(mg/kg) ≤ 5 Appendix A A.7
Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.8
Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.9
Loss on drying, w /% ≤ 8.0 Appendix A A.10
Loss on ignition, w /% 8.0 ~ 13.0 Appendix A A.11
pH (20% slurry) 6.5 to 10.5 A.12 in Appendix A
Appendix A
(Normative)
Testing method
A.1 Warning
The standard test methods required for use of some strong acid, when used, be careful to avoid splashing on the skin! As should be immediately splashed on the skin
Rinsed with water, severe cases should be treated immediately. When using a volatile acid, to be carried out in a fume hood.
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 in
Three water regulations. 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 of HG/T 3696.3 of preparation.
A.3 Identification Test
A.3.1 Identification of silicate
The 0.5 g sample was mixed with 2.5 g of anhydrous potassium carbonate, on the electric heating in a platinum crucible to melt the mixture, cooled, 5 mL
Water and let stand 3 min, the crucible plus micro heat, add 50 mL of water to dissolve. Completely transferred to a beaker, was added dropwise a solution of hydrochloric acid (11) to airless
Bulbs, add 10 mL of hydrochloric acid, evaporated to dryness on a steam bath to cool. Was added 20 mL of water, filtered boiling, insoluble gel residue
Used to identify silicon. A filtrate is used to identify the test solution of aluminum.
The gelatinous residue was taken platinum crucible, carefully add 5 mL of hydrofluoric acid. The precipitate was dissolved. Heating, placed in the vapor above the crucible
A glass rod moistened with a drop of water, the water droplets become cloudy.
A.3.2 Identification of aluminum ions
Was added dropwise in the test solutions A (A.3.1) in aqueous ammonia solution (11), a white gelatinous precipitate, addition of excess aqueous ammonia solution, no precipitate
Dissolved. Was added dropwise a solution of sodium hydroxide (40 g/L) to give a white gelatinous precipitate, the precipitate dissolved when added in excess.
A.3.3 Identification of sodium ions
Wetting platinum wire with hydrochloric acid, colorless to burn in the flame, then dipped a little in the test solution combustion flame, the flame that is dark yellow.
A.4 Determination of silica
A.4.1 Method summary
Silica in the sample with hydrofluoric acid forming volatile matter by burning volatile, by determining the mass difference before and after ignition calculated silica
content.
A.4.2 Reagents and materials
A.4.2.1 sulfuric acid.
A.4.2.2 hydrochloric acid.
A.4.2.3 hydrofluoric acid.
A.4.3 Instruments and Equipment
High-temperature furnace. temperature can be maintained at 900 ℃ ± 25 ℃.
A.4.4 Analysis step
Weigh was 105 ℃ ± 2 ℃ bake a sample of about 0.5 g 2 h, to the nearest 0.000 2 g, into a 200 mL beaker with a small amount of water will
Wash the beaker wall. Added 30 mL and 15 mL of sulfuric acid, hydrochloric acid, in a hood on a hot plate heated until white smoke is generated, added 15 mL After cooling
Hydrochloric acid, heated again to generate white smoke. Evaporated to about 10 mL solution was left and cooled, was added 70 mL of water, filtered using filter paper, and dried
Hot water and sediment filter.
The filter paper and transferred to precipitate a platinum crucible, burning to constant mass at 900 ℃ ± 25 ℃, saying its quality. Residue was moistened with water,
8 drops of sulfuric acid was added followed by 15 mL of hydrofluoric acid, heated on a hot plate to produce white smoke. Steam until nearly dry, add 5 mL of water. After cooling, 3
Drops of sulfuric acid and 10 mL of hydrofluoric acid, hot plate evaporation to near dryness on a hot plate heated to white smoke rush the net. The crucible in
900 ℃ ± 25 ℃ to constant burning quality. The mass loss after hydrofluoric acid is added to the sample quality silica (SiO2) taken.
A.4.5 Calculation Results
Silica content of silicon dioxide (SiO2) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated.
0211 × - = m
mmw (A.1)
Where.
1m - for the first time after a constant burning quality to value the quality of the crucible and precipitate in grams (g);
2m - the second (after adding the hydrofluoric acid treatment) value to the quality of constant quality after burning crucible and precipitate in grams (g);
m - mass of the sample value in units of 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 0.1%.
A.5 Determination of aluminum oxide
A.5.1 Method summary
The samples were processed, an excess of disodium edetate solution in the test solution, and aluminum complex, with xylenol orange as indicator
Zinc chloride standard titration solution titrate excess of disodium edetate solution.
A.5.2 Reagents and materials
A.5.2.1 perchloric acid.
A.5.2.2 hydrofluoric acid.
A.5.2.3 hydrochloric acid.
A.5.2.4 ammonia.
A.5.2.5 hydrochloric acid solution. 11.
A.5.2.6 disodium EDTA standard titration solution. c (EDTA) = 0.01 mol/L.
A.5.2.7 zinc chloride standard titration solution. c (ZnCl2) = 0.01 mol/L.
A.5.2.8 xylenol orange indicator solution. 5 g/L.
A.5.3 Analysis step
Weigh was 105 ℃ ± 2 ℃ bake a sample of about 0.3 g 2 h, to the nearest 0.0002 g, into a platinum crucible, with 8 to 10 drops of water dripping Run
wet. Perchloric acid was added 15 mL and 10 mL of hydrofluoric acid, in a hood on a hotplate until generate a large amount of perchloric acid white smoke, steam to near
Dry After cooling 10 mL of hydrofluoric acid and heated to generate dense white smoke again evaporated to near dryness, added 4 mL of hydrochloric acid was dissolved by heating,
After cooling completely transferred to a 250 mL volumetric flask, wash with hot water in a platinum crucible and the lotion into the volumetric flask and dilute to the mark with water, shake
uniform.
Pipette 50.00 mL of the solution into 250 mL conical flask, add water to 100 mL, was added 20.00 mL disodium edetate
Standard Solution, add 3 to 4 drops drops xylenol orange indicator solution, the solution was adjusted with ammonia reddish. 1min boiling on a hot plate, remove the cold
But (if the excess ammonia, the solution was adjusted with hydrochloric acid solution was bright yellow, then the excess two drops). Titration with zinc chloride standard titration solution to the solution from
Yellow to reddish color is the end. While the same treatment the blank test solution.
In addition to the blank test without the sample, the type and amount of addition of reagents and other operating and measured in the same test.
A.5.4 Calculation Results
Aluminum oxide content of aluminum oxide (Al2O3) mass fraction w2 and its value is expressed in%, according to formula (A.2) Calculated.
()
2 ××
- =
cMVVw
(A.2)
Where.
Numerical zinc chloride standard titration solution volume consumed V0-- blank test, in milliliters (mL);
Numerical zinc chloride standard titration solution volume consumed V1-- titration, in milliliters (mL);
c - accurate zinc chloride standard titration solution concentration value in units of moles per liter (mol/L);
Numerical m-- sample mass, expressed in grams (g);
(1/2Al2O3) molar mass of aluminum oxide M-- value, in units of grams per mole (g/mol) (M = 50.98).
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%.
A.6 Determination of sodium oxide
A.6.1 Method summary
Sample after treatment, the sample solution is introduced into the flame emission meter, an aerosol spray system introduced in the flame, the flame will again rely on
Sample solution was evaporated, and excited atoms generated spectrum, spectrum sodium atoms occur at characteristic wavelengths 589.0nm under its line intensities and sodium oxide
Proportional content, compared with standard series quantitation.
A.6.2 Reagents and materials
A.6.2.1 perchloric acid.
A.6.2.2 hydrofluoric acid.
A.6.2.3 hydrochloric acid.
A.6.2.4 Sodium standard solution. 1 mL solution of sodium (Na) 0.1 mg.
Pipette 10.00 mL sodium standard solution according to HG/T 3696.2 prepared, placed in 100mL flask, diluted with water to the mark.
The solution was prepared prior to use.
A.6.2.5 sulfate standard solution. 1 mL solution containing sodium sulfate (Na2SO4) 100 mg.
Accurately weighed 10.00 g after 95 ℃ ~ 105 ℃ drying 2 h, cooled to room temperature and anhydrous sodium sulfate, dissolved in water and transferred to 100 mL capacity
Volumetric flask, dilute to the mark, shake, placed in the refrigerator to save, backup.
A.6.2.6 two water. in line with GB/T 6682-2008.
A.6.3 Instruments and Equipment
A.6.3.1 flame photometer.
A.6.3.2 conductivity meter.
A.6.4 Analysis step
A.6.4.1 Determination of sodium correction
A.6.4.1.1 Preparation of sample solution
Weigh the sample was 105 ℃ ± 2 ℃ bake 2 h of 12.5 g, accurate to 0.0002 g, placed in 400 mL water beaker 240 mL,
High speed stirring for at least 5 min. The mixture was completely transferred to 100 mL volumetric flask, dilute to the mark, shake.
A.6.4.1.2 Preparation of standard solution
Pipette standard solution of sodium 0.00 mL, 0.50 mL, 1.00 mL, 2.00 mL, 5.00 mL, were placed in 100 mL volumetric flask,
Diluted with water to the mark.
A.6.4.1.3 Determination
The sample and standard solution electric conductivity detected. In the electrical conductivity of the vertical axis, the quality of sodium (mg) as abscissa, work
curve.
A.6.4.1.4 Calculation Results
Correction sodium content of sodium oxide (Na2O) mass fraction F and its value is expressed in%, according to formula (A.3) Calculated.
010,437.0
1 ×× =
mF
(A.3) where.
Numerical solution m1-- quality sample isolated from the working curve of sodium in milligrams (mg);
Numerical m-- sample mass, expressed in grams (g);
0.437-- sodium sulfate sodium oxide conversion factor.
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%.
A.6.4.2 Preparation of sample solution
Weigh the sample was ± bake about 0.3 g 105 ℃ 2 ℃ 2h, and accurate to 0.000 2 g, placed in a platinum crucible, with 8 to 10 drops of water dripping wet. plus
Into 15 mL of perchloric acid and 10 mL of hydrofluoric acid, in a hood on a hot plate heated until white smoke generates a lot of perchloric acid, evaporated to near dryness, cooling
After 10 mL of hydrofluoric acid, was again heated to generate dense white fumes evaporated to near dryness, was added 4 mL of hydrochloric acid, dissolved by heating, cooled and finished
Full transferred to a 500 mL volumetric flask, wash with hot water in a platinum crucible and lotion incorporated into the flask, diluted with water to the mark. Pipette on
10.00 mL of said solution into 100 mL volumetric flask, dilute to the mark, shake. While the same treatment the blank test solution.
A.6.4.3 Preparation of the blank test solution
In addition to the blank test without the sample, the type and amount of addition of reagents and other operations of the same prepared sample solution.
A.6.4.4 Preparation of standard solutions
Pipette sodium standard solution 0.00 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, were placed in 100 mL volumetric flask, dilute with water
Release to the mark.
A.6.4.5 Determination
The test solution and standard solution at a wavelength of 589.0 nm at zero adjustment water was measured line intensities. Quality of sodium (mg) is a cross
Coordinates corresponding to the line intensity as the ordinate, drawing working curve.
A.6.5 Calculation Results
Sodium oxide content of sodium oxide (Na2O) mass fraction w3 and its value is expressed in%, according to formula (A.4) calculated as follows. ()
mmw - ××
× - = 0
10348.1 301
3 (A.4)
Where.
Numerical quality test solution m1-- isolated from the working curve of sodium in milligrams (mg);
Numerical quality blank solution m0-- isolated from the working curve of sodium in milligrams (mg);
Numerical m-- sample mass, expressed in grams (g);
1.348-- sodium sodium oxide conversion factor;
F-- determined according to A.6.4.1 correction sodium content, expressed as% values.
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%.
A.7 Determination of Lead
A.7.1 Reagents and materials
A.7.1.1 4- methyl amyl ketone -2 (MIBK).
A.7.1.2 hydrochloric acid solution. 120.
A.7.1.3 ammonia solution. 11.
A.7.1.4 ammonium sulfate solution. 300 g/L.
Weigh 30g of ammonium sulfate [(NH4) 2SO4], dissolved in water and add water to 100 mL.
A.7.1.5 ammonium citrate solution. 250 g/L.
Weigh 25g of ammonium citrate, dissolved in water and add water to 100 mL.
A.7.1.6 bromothymol blue solution. 1 g/L.
A.7.1.7 diethyl dithiocarbamate (DDTC) solution. 50 g/L.
A.7.1.8 Weigh 5 g diethyl dithiocarbamate, dissolved in water and add water to 100 mL.
A.7.1.9 Lead standard solution. 1 mL solution containing lead (Pb) 0.001 mg.
Pipette 1.00 mL of lead standard solution according to HG/T 3696.2 prepared, placed in 1000 mL volumetric flask, dilute to the mark, shake.
The solution was prepared prior to use.
A.7.1.10 two water. in line with GB/T 6682-2008.
A.7.2 Instruments and Equipment
Atomic absorption spectrophotometer.
A.7.3 Analysis step
A.7.3.1 Preparation of test solution
Weigh 10.00 g ± 0.01 g sample was placed in 250 mL beaker, add 50 mL of hydrochloric acid solution, cover the surface of the dish, slowly heated to
Boiling and kept boiling for 15 min, cooled, insolubles were allowed to stand for settling. The solution was filtered to a 100 mL volumetric flask three times with hot water clean
Wash the beaker (try to make insolubles remain in the beaker) per 10 mL of water, and finally with 15 mL of hot water to clean the filter and the filtrate was incorporated into 100 mL
Volumetric flask. After cooling, diluted with water to the mark, shake, backup, keep this solution as filtrate B, for lead content of arsenic, heavily
Determination of the genus.
Pipette pipette 10.00 mL filtrate B, placed in 125 mL separatory funnel, add water to make 60 mL. Add 2 mL ammonium citrate solution
Liquid drops 3 to 5 drops of bromothymol blue indicator solution, the pH is adjusted with ammonia solution from yellow to blue, add 10 mL of ammonium sulfate solution, 10 mL of diethyl
Dithiocarbamate (DDTC) solution, shake. Place about 5 min, transferred 10.00 mL 4- methyl amyl ketone -2 (MIBK), severe vibration
Shake extract 1 min, after standing layer, the aqueous layer was discarded, the 4-methyl amyl ketone -2 (MIBK) layer into a 10 mL stoppered graduated tube, and set aside.
A.7.3.2 blank test solution.
In addition to the blank test without the sample, the preparation of the same kind and amount of the test solution and other operations and the addition of reagents.
A.7.3.3 Preparation of standard reference solution than
Pipette respectively, 0.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL of lead standard solution, placed in five 125 mL separating funnel
, Each 5 mL of hydrochloric acid solution was added, according to 7.3.1 from "additional water to 60 mL" start simultaneously with the sample solution is treated similarly.
A.7.3.4 Determination
The test solution and standard solution at a wavelength of 283.3 nm at water zero adjustment, the absorbance was measured. Quality of lead (mg) is a cross
Coordinates corresponding absorbance as the ordinate, drawing working curve.
A.7.4 Calculation Results
Lead in lead (Pb) mass fraction w4 and its value in mg/kg according to formula (A.5) Calculated.
4 ××
- = -m
mmw (A.5)
Where.
m1 - Numerical test solution isolated from the working curve lead mass in milligrams (mg);
m0 - value blank test solution isolated from the working curve lead 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 1 mg/kg.
A.8 Determination of Arsenic
A.8.1 Reagents and materials
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
Pipette 10.00 mL filtrate B (A.7.3.1), placed in a conical flask arsenic measuring apparatus, the following according to GB/T 5009.76-2003 11th
Operation.
Limits formulated solution. Pipette 3.00 mL of arsenic standard solution (1 mL solution containing 1.0 μgAs), with the same sample at the same time
Management.
A.9 heavy metals (Pb) Determination
A.9.1 Reagents and materials
A.9.1.1 hydrochloric acid solution. c (HCl) ≈0.5 mol/L.
A.9.1.2 hydrochloric acid solution. 120.
A.9.1.3 ammonia solution. 13.
A.9.1.4 nitric acid solution. 19.
A.9.1.5 phenolphthalein indicator solution.
A.9.1.6 sodium sulfide glycerol solution.
A.9.1.7 acetate buffer solution. pH = 3.5.
Weigh 25.0 g ammonium acetate dissolved in 25 mL of water, add 45 mL of hydrochloric acid solution (A.9.1.1), with a hydrochloric acid solution (A.9.1.2) or ammonia
The pH was adjusted to 3.5 of 5 (pH meter), diluted with water to 100 mL.
A.9.1.8 Lead standard solution. 1 mL solution containing lead (Pb) 0.001 mg;
Pipette 1.00 mL of lead standard solution according to HG/T 3696.2 prepared, placed in 1000 mL volumetric flask, dilute to the mark, shake.
The solution was prepared prior to use.
A.9.2 Analysis step
A.9.2.1 A tube. pipette 10.00 mL lead standard solution was placed in 50 mL colorimetric tube, add 5 mL of hydrochloric acid (A.9.1.2), add water to 25 mL,
Add 1 drop of phenolphthalein indicator solution was added dropwise a solution of hydrochloric acid (A.9.1.2) of aqueous ammonia solution or pink just faded, then add 5 mL of acetic acid
Buffer solution, mix and set aside.
A.9.2.2 B, C Pipe. Pipette 10.00 mL, respectively filtrate B (A.7.3.1) into two 50 mL colorimetric tubes, each 1 drop of phenolphthalein indicator
Liquid, after dropping ammonia solution to pink, then dropping hydrochloric acid solution (A.9.1.2) and to the solution faded pink, add water to 25 mL, shake
uniform. 10.00 mL of lead standard solution C tube moved. B, C, respectively, the tube was added 5 mL of acetate buffer solution, mix and set aside.
A.9.2.3 Limited colorimetric. each tube 2 drops of sodium sulfide glycerol solution, and add water to 50 mL volume, and mix in a dark place 5 min
After observation on white background, B can not be deeper than the color tube A tube of color, C color shall A tube tube color or fairly deep in the tube A
Chromaticity.
A.10 Determination of loss on drying
A.10.1 instruments and equipment
A.10.1.1 electric oven. capable of controlling the temperature of 105 ℃ ± 2 ℃.
A.10.1.2 porcelain crucible.
A.10.2 Analysis steps
Use to bake constant quality porcelain crucible at 105 ℃ ± 2 ℃, weigh about 5 g samples, accurate to 0.0002 g. At 105 ℃ ± 2 ℃ Power
Bake in hot oven thermostat 2 h, cooled call quality.
A.10.3 Calculation Results
Loss on drying mass fraction w5 and its value is expressed in%, according to formula (A.6) Calculated.
()
0125 × - = m
mmmw
(A.6)
Where.
1m - Numerical crucible mass in grams (g);
At 2m --105 ℃ ± 2 ℃ bake 2 h after the value of the crucible and the sample mass, in grams (g);
m - mass of the sample value in units of 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.11 Determination of loss on ignition
A.11.1 instruments and equipment
A.11.1.1 temperature furnace. to control the temperature 900 ℃ ± 25 ℃.
A.11.1.2 porcelain crucible.
A.11.2 Analysis steps
Use to bake constant quality porcelain crucible at 900 ℃ ± 25 ℃, weigh about 5 g samples, accurate to 0.0002 g. At 900 ℃ ± 25 ℃
High-temperature furnace burning to a constant quality.
A.11.3 Calculation Results
LOI mass fraction w6 and its value is expressed in%, according to formula (A.7) calculated as follows.
()
0136 × - = m
mmm
w (A.7)
Where.
1m - Numerical crucible mass in grams (g);
3m --900 ℃ ± 25 ℃ high temperature furnace burning to the value of the crucible and the sample quality after quality constant in units of grams (g);
m - mass of the sample value in units of 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.12 pH measurement
A.12.1 instruments and equipment
pH meter. Indexing is 0.02.
A.12.2 Analysis steps
Weigh 20.00 g ± 0.01 g sample was placed in 250 mL beaker. Dissolved in 100 mL of carbon dioxide-free distilled water. Stirring to form
Homogeneous aqueous slurry, according to the provisions of GB/T 9724-2007 Determination of pH of the solution.
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