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GB 25580-2010: The national food safety standards of food additives stable chlorine dioxide solution
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The national food safety standards of food additives stable chlorine dioxide solution
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GB 25580-2010
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Basic data | Standard ID | GB 25580-2010 (GB25580-2010) | | Description (Translated English) | The national food safety standards of food additives stable chlorine dioxide solution | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 9,960 | | 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 food additives carbonate absorption by chlorine dioxide system was the food additive stable chlorine dioxide solution. The product is in the use of food additives hydrochloric acid activation. | GB 25580-2010: The national food safety standards of food additives stable chlorine dioxide solution
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The national food safety standards of food additives stable chlorine dioxide solution
National Food Safety Standard
Food Additives stable chlorine dioxide solution
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 stable chlorine dioxide solution
1 Scope
This standard applies to food additives carbonate absorbed by the food additive stable chlorine dioxide solution of chlorine dioxide system was. this product
When using activation with hydrochloric acid food additives.
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 Technical requirements
3.1 Sensory requirements. comply with Table 1.
Table 1 Sensory requirements
Project requires test methods
Colorless or yellow color. Take the right amount of sample is placed in a colorimetric tube and observed under natural light color
Chak and texture. State organization transparent liquid without suspension.
3.2 Physical indicators. to comply with Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Chlorine dioxide, w /% ≥ 2.0 Appendix A A.4
Density, ρ20/(g/mL) 1.020 ~ 1.060 A.5 in Appendix A
pH 8.2 ~ 9.2 in Appendix A A.6
Arsenic (As)/(mg/kg) ≤ 1 Appendix A A.7
Heavy metals (Pb)/(mg/kg) ≤ 5 Appendix A A.8
Methanol, ρ/(g/100mL) ≤ 0.04 A.9 in Appendix A
Appendix A
(Normative)
Testing method
A.1 Warning
Reagents of this standard test method for use in corrosive, the operator must be careful! As splashed on the skin should immediately wash with water,
In severe cases, seek immediate medical attention. When using flammable, do not use open flame heating.
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 hydrochloric acid solution. 1 + 2.
A.3.1.2 calcium chloride solution. 100 g/L.
A.3.2 Analysis step
A.3.2.1 Identification of sodium ions
Infiltration of platinum wire with hydrochloric acid to colorless in the first combustion colorless flame. Then dipped a little test solution, the colorless flame combustion, through cobalt glass
Glass observe the flame was bright yellow.
A.3.2.2 Identification of carbonate
Calcium chloride solution was added in the test solution, a white precipitate. The precipitate was dissolved in hydrochloric acid.
A.3.2.3 Identification chlorine dioxide
Yellow gas can produce hydrochloric acid solution in the test solution, the test solution while also yellow.
Determination of chlorine content A.4 dioxide
A.4.1 Iodimetry (Arbitration Act)
A.4.1.1 Method summary
The first step in pH≤2 when masked with malonic hypochlorite (ie chlorine) interference sample chlorine dioxide and chlorite all
Reaction with potassium iodide, sodium thiosulfate standard solution titration generated iodine. The second step to take another sample, the solution was adjusted pH≤2, nitrogen catch
To chlorine and chlorine dioxide in the sample chlorite and potassium iodide, sodium thiosulfate solution titrated with standard iodine generated. By-step anti
We shall calculate the difference between the actual content of chlorine dioxide in the sample.
A.4.1.2 Reagents and materials
A.4.1.2.1 purity nitrogen.
A.4.1.2.2 hydrochloric acid solution. 1 + 4.
A.4.1.2.3 potassium iodide solution. 100 g/L.
A.4.1.2.4 sulfuric acid solution. 1 + 8.
A.4.1.2.5 malonic acid. 100 g/L.
A.4.1.2.6 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1 mol/L.
A.4.1.2.7 starch indicator solution. 5g/L.
A.4.1.3 analysis step
A.4.1.3.1 Preparation of test solution A
Weigh approximately 10 g samples, accurate to 0.000 2 g, was transferred to a 50mL volumetric flask, dilute to the mark, shake. The solution is a test
Solution A, used to determine the chlorine dioxide content.
A.4.1.3.2 Determination
Pipette with a pipette respectively 10.00mL test solution A, has been previously placed in two 50mL of water was added iodine bottle, were added 2mL
Hydrochloric acid solution, water seal stamped in first and second place immediately after 30min measured.
The first step. In a flask was added 3 mL iodine solution malonate, dark place to stand 3 min. Sulfuric acid solution was added 10 mL, 10 mL
Potassium iodide solution, mix, dark place to stand 5 min. Standard titration with sodium thiosulfate solution titration, 1 mL of starch indicator near the end
Solution, continue titration to the disappearance of the blue just as the end point, the volume of consumption recorded for V1.
Step two. another iodine bottle placed in a ventilated hood, which leads to high purity nitrogen gas is blown to the yellow-green disappeared after blowing 20 min. plus
Malonate into 3 mL solution, placed in the dark standing 3 min. Sulfuric acid solution was added 10 mL, 10 mL potassium iodide solution, mix, placed in the dark quiet
Set 5 min. Standard titration with sodium thiosulfate solution titration, 1 mL was added near the end of starch indicator solution and continue to drop until the end of the blue just disappears
Point, record the consumption volume is V2.
A.4.1.4 Calculation Results
Chlorine dioxide content of chlorine dioxide (ClO2) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated.
() 05010
] 1000 /) [(21
1 ××
- =
cMVVw (A.1)
Where.
V1-- first step titration solution consumption of sodium thiosulfate standard titration solution volume value in milliliters (mL);
V2-- second step titration solution consumption of sodium thiosulfate standard titration solution volume value in milliliters (mL);
c - accurate thiosulfate standard titration solution concentration value in units of moles per liter (mol/L);
Numerical m-- sample mass, expressed in grams (g);
M-- chlorine dioxide (1/5ClO2) molar mass values, in units of grams per mole (g/mol) (M = 13.49).
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.02%.
A.4.2 spectrophotometry
A.4.2.1 Method summary
Chlorine dioxide has a characteristic absorption at 430nm, measured using spectrophotometry.
A.4.2.2 Reagents and materials
A.4.2.2.1 chlorine-free distilled water.
Sodium sulfite in water to DPD chlorine assay reagent check not develop a color, and then distillation, collecting distillate.
A.4.2.2.2 hydrochloric acid solution. 1 + 4.
A.4.2.2.3 chlorine dioxide standard stock solution.
Preparation. A bottle placed in 300 mL of water, the A glass bottle with an air compressor connecting one end, and another glass bottle B is connected. B
Bottle of high strength borosilicate glass, glass bottle has three; the first to root cuttings from the bottom of a glass bottle at 5 mm for the introduction of air; the second root
Then dropping funnel, the lower end of the hopper extends below the surface; a third liquid leaving the lower end, the upper end of the bottle and the C phase. 10 g of sodium chlorite dissolved in 750 mL
Bottle of water and poured into B; sulfuric acid solution containing 1 + 10 in 20 mL separatory funnel. C bottled saturated solution of sodium hypochlorite. D 2 L bottles
Borosilicate glass collection bottle, the bottle containing 1500 mL of water, chlorine dioxide to absorb what happened, residual gas discharged from the exhaust pipe. The entire device should be placed
In a fume hood (see Figure A.1).
Figure A.1 chlorine dioxide absorbing device of FIG.
Start air compressor, air equalization through the entire apparatus. Every 5 min from the separating funnel was added 5 mL of sulfuric acid solution was added after the last
After a sulfuric acid solution, air traffic continues to 30 min. Yellow chlorine dioxide standard solution to obtain a discharge in a brown bottle, stored at 4 ℃, which
Concentration should be 250 mg/L ~ 600 mg/L.
A.4.1 according to the method prescribed stock solution of chlorine dioxide in the chlorine dioxide concentration was measured (should all stock solution concentration before each use
Determination).
A.4.2.2.4 chlorine dioxide standard solution. 1mL solution containing chlorine dioxide (ClO2) 0.25 mg.
Determination of the concentration of stock solution of chlorine dioxide, chlorine dioxide absorb a certain amount of standard stock solution was diluted with distilled water without chlorine. The solution
That match was ready to use.
A.4.2.3 analysis step
Drawing A.4.2.3.1 calibration curve
Were taken 0.00 mL, 10.00 mL, 20.00 mL, 40.00 mL, 60.00 mL, 80.00 mL, 100.00 mL standard solution of chlorine dioxide
Liquid, placed in seven 100 mL volumetric flask, chlorine-free distilled water to the mark. At 430 nm wavelength, the choice of 1 cm cuvette,
Chlorine-free distilled water to zero, the absorbance is measured.
Subtracting the absorbance of the reagent blank solution from the absorbance of each standard solution, the quality of chlorine dioxide (mg) as abscissa, corresponding to suck
Photometric ordinate, drawing working curve.
A.4.2.3.2 Determination
Weigh 0.7 g samples, accurate to 0.000 2 g, was added 10 mL hydrochloric acid solution was transferred to a 100 mL volumetric flask, dilute with distilled water without chlorine
Release to the mark. At 430 nm wavelength, the choice of 1 cm cuvette, chlorine-free distilled water to zero, the absorbance is measured. From the working curve
Isolated quality chlorine dioxide test solution.
A.4.2.4 Calculation Results
Chlorine dioxide content of quality chlorine dioxide (ClO2) fraction w1 and its value is expressed in%, according to formula (A.2) Calculated.
1 ×× =
mw (A.2)
Where.
Test solution m1-- Richard from the working curve of chlorine dioxide mass value, 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 parallel determination of the absolute difference is not more than 0.02%.
A.5 Determination of density
A.5.1 Instruments and Equipment
2.3.3.2 The provisions of GB/T 4472-1984.
A.5.2 Analysis step
2.3.3.3 The provisions of GB/T 4472-1984.
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 0.003 g/cm3.
A.6 pH measurement of
A.6.1 Instruments and Equipment
With GB/T 9724-2007 of Chapter 5.
A.6.2 Analysis step
The sample was poured into a beaker, the following according to GB/T 9724-2007 Determination of Chapter 6.
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 pH units.
A.7 Determination of Arsenic
Weigh 1.00 g ± 0.01 g sample was placed in 100mL beaker, add hydrochloric acid solution (1 3) 8 mL. Placed on the electric stove to boil nearly dry,
Remove cooling to room temperature, add a small amount of water, as the test solution.
Limits formulated solution. Pipette 1.00 mL of arsenic standard solution [1mL solution containing 1.0μg arsenic (As)], the following according to GB/T 5009.76
Chapter 11 -2003 operations from "were placed in a conical flask" to start the measurement.
A.8 Determination of Heavy Metals
Weigh 1.00 g ± 0.01 g sample was placed in 100 mL beaker, add hydrochloric acid solution (1 3) 8mL, placed on the electric stove to boil nearly dry,
Remove to cool to room temperature, add a little water and transferred to 50 mL colorimetric tube, add 1 drop of phenolphthalein indicator solution with aqueous ammonia solution and hydrochloric acid solution and dissolved
pH of the solution is neutral (phenolphthalein just faded red) as the test solution.
Pipette Pipette 0.50mL lead standard solution [1 mL solution containing 0.01mg of lead (Pb)] as a standard, the following according to GB/T 5009.74-2003
Chapter 6 is measured.
A.9 Determination of Methanol
A.9.1 Reagents and materials
A.9.1.1 potassium permanganate - phosphoric acid solution.
Said 3 g of potassium permanganate, phosphoric acid Add 15 mL of water and 70 mL of the mixture, water was added to dissolve 100 mL. Store in a brown bottle
Inside.
A.9.1.2 oxalic acid - sulfuric acid solution.
Weigh 5 g or 7 g of anhydrous oxalic acid containing two crystal water of oxalic acid, sulfuric acid solution with 1 + 1 was dissolved and diluted to 100 mL.
A.9.1.3 magenta - sulfite solution.
After weighing 0.1 g of fuchsin small study, graded by adding a total of 80 ℃ water 60 mL, grinding with addition of water to dissolve, with the upper pipette
The solution was filtered in 100 mL volumetric flask. After cooling, add 100 g/L sodium sulfite solution 10 mL, add 1 mL of hydrochloric acid, add water to the mark
Mix to stand overnight. Such as a solution color, plus a small amount of activated carbon were filtered after stirring, stored in a brown bottle, set in dark place, the solution was red
It should be reconstituted.
A.9.1.4 methanol standard stock solution. 1 mL solution containing methanol (CH3OH) 10 mg.
Weigh 1.000 g of methanol, placed in 100 mL volumetric flask, diluted with water to the mark.
A.9.1.5 methanol standard solution. 1 mL solution containing methanol (CH3OH) 1 mg.
Pipette pipette 10.00 mL of methanol stock standard solution (A.9.1.4), placed in 100mL flask, diluted with water to the mark.
This solution is using now.
A.9.2 Analysis step
Pipette Pipette 1.00 mL sample was placed in 25 mL with stopper colorimetric tube, add water to 15 mL, as the test solution.
Limits formulated solution. Pipette 0.40 mL of methanol standard solution (A.9.1.5), placed on the other colorimetric tube, add water to 15 mL.
In two colorimetric tubes were added 2 mL of potassium permanganate - phosphoric acid solution, mixing, placing 10 min. Added 2 mL of oxalic acid - sulfuric acid solution,
Mix to make it fade, then add 5 mL magenta - sulfite solution was diluted with water to the mark. 20 ℃ above was allowed to stand at 30 min, the sample
The form can not be deeper than the color standard.
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