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GB 1886.221-2016 English PDF

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GB 1886.221-2016: Food additive -- Ponceau 4R Aluminum lake
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Basic data

Standard ID GB 1886.221-2016 (GB1886.221-2016)
Description (Translated English) Food additive -- Ponceau 4R Aluminum lake
Sector / Industry National Standard
Classification of Chinese Standard X42
Word Count Estimation 9,980
Date of Issue 2016-08-31
Date of Implementation 2017-01-01
Older Standard (superseded by this standard) GB 4480.2-2001
Regulation (derived from) Announcement of the State Administration of Public Health and Family Planning 2016 No.11
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 1886.221-2016: Food additive -- Ponceau 4R Aluminum lake

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(Food safety national standard - Food additive - Carmine aluminum lake) National Standards of People's Republic of China National Food Safety Standard Food additives carmine aluminum lake Issued on. 2016-08-31 2017-01-01 implementation People's Republic of China National Health and Family Planning Commission released

Foreword

This standard replaces GB 4480.2-2001 "food additive carmine aluminum lake." This standard compared with GB 4480.2-2001, the main changes are as follows. --- Standard name was changed to "national food safety standards for food additives carmine aluminum lake"; --- Modify the scope; --- Increasing the chemical name; --- Modify the molecular weight; --- Index name Appearance modify sensory requirements; --- Modify the content of the indicator; --- Hydrochloric acid and ammonia water insolubles Index name changed to hydrochloric acid insoluble matter was revised test methods; --- Heavy Metals (as Pb) Index name changed to lead, to modify the index requirements and test methods; --- Remove the loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 to count), Vice-dye, barium index requirements and inspection method; --- Revised test methods for arsenic. National Food Safety Standard Food additives carmine aluminum lake

1 Scope

This standard applies to food additives and carmine aluminum lake as raw material and prepared food additive carmine aluminum lake.

2 Chemical name and relative molecular mass

2.1 Chemical Name 1- (4'-sulfo-1'-naphthyl) azo-2-naphthol-6,8-disulfonic acid trisodium salt of aluminum lakes. 2.2 relative molecular weight 631.51 (Carmine dollars) (according to 2013 international relative atomic mass).

3 Technical requirements

3.1 Sensory requirements Sensory requirements shall comply with the requirements of Table 1. Table 1 Sensory requirements Project requires test methods Red color State powder Take appropriate sample is placed in a clean, dry white porcelain dish, self Under natural light, observe its color and status 3.2 Physical and Chemical Indicators Physical and chemical indicators should be consistent with the provisions of Table 2. Table 2. Physical and chemical indicators Item Index Test Method Carmine content (sodium salt dollars), w /% in line with claims in Appendix A A.4 Hydrochloric acid insoluble matter, w /% ≤ 0.5 A.5 in Appendix A Arsenic (As)/(mg/kg) ≤ 3.0 GB 5009.11 or GB 5009.76 Lead (Pb)/(mg/kg) ≤ 5.0 GB 5009.12 or GB 5009.75

Appendix A

Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, the operation should take appropriate safety and health practices. A.2 General Provisions This standard reagents and water in the absence of other specified requirements, refer to the three water analytical reagent and GB/T 6682 regulations. test Used in the standard solution, standard solution for measuring impurities, formulations and products, did not indicate when the other requirements according to GB/T 601, GB/T 602, GB/T 603 provisions of the preparation. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 sulfuric acid solution. 120. A.3.1.2 hydrochloric acid solution. 14. A.3.1.3 sodium hydroxide solution. 100g/L. A.3.1.4 ammonium acetate solution. 1.5g/L. A.3.1.5 activated carbon. A.3.2 Instruments and Equipment A.3.2.1 Spectrophotometer. A.3.2.2 cuvette. 10mm. A.3.3 Analysis step A.3.3.1 color reaction Weigh about 0.1g sample, add 5mL sulfuric acid solution continuously shaken in a water bath and heated for about 5min, red solution, after cooling, to take on Clarification layer drops 2 drops to 3 drops, add 5mL water, still on red. A.3.3.2 aluminum reaction Weigh about 0.1g sample, add 5mL hydrochloric acid solution and heated in a water bath, so that most of the dissolved. Add 0.5g of activated carbon, shake well Uniform, cooled and filtered. Take a colorless filtrate, add sodium hydroxide solution and after rendering aluminum reaction. A.3.3.3 maximum absorption wavelength Weigh about 0.1g sample, add sulfuric acid solution 5mL, heated and dissolved in a water bath after the full mix, add ammonium acetate solution equipped to 100mL. Centrifuged the solution is not clarified. Then take this solution 1mL ~ 5mL, plus ammonium acetate solution equipped to 100mL. So that the absorbance measurement Degree in the range of 0.3 to 0.7, the maximum absorption wavelength of this solution is 505nm ~ 510nm. A.4 Determination of the content of carmine A.4.1 Titanium trichloride titration (Arbitration Act) A.4.1.1 Method summary In acidic medium, Carmine structure azo group is reductive decomposition of titanium trichloride, titanium trichloride consumption according to standard titration solution, Calculate the content. A.4.1.2 Reagents and materials A.4.1.2.1 trisodium citrate. A.4.1.2.2 titanium trichloride standard titration solution. c (TiCl3) = 0.1mol/L (now with the existing, method of preparation see Appendix B). A.4.1.2.3 sulfuric acid solution. 120. A.4.1.2.4 Carbon dioxide. content ≥99%. A.4.1.3 instruments and equipment Titanium trichloride titration apparatus shown in Figure A.1. Explanation. A --- conical flask (a 500 mL); B --- brown burette (50mL); C --- package under glass bottle of black paper (2000mL); D --- containing ferrous sulfate and ammonium carbonate equivalent mixture container (5000mL); E --- piston; F --- bottles; G --- washing bottle filled with water. Figure A.1 apparatus of FIG titanium trichloride titration A.4.1.4 analysis step Weigh about 2g sample (accurate to 0.0001g), placed in 500mL conical flask, sulfuric acid solution 20mL and 50mL freshly boiled Of water and cooled to room temperature, shaking constantly heated water bath until dissolved, add 15g trisodium citrate and 150mL of freshly boiled water, shaking After dissolution, according to Figure A.1 instrument installed at the level of carbon dioxide introduced into the same time, heated to boiling, and treated with titanium trichloride standard titration solution drop Given the inherent color of the sample solution to disappear as the end point. A.4.1.5 Calculation Results Carmine content mass fraction w1, according to equation (A.1) Calculated. w1 = V × c × M m × 1000 × 4 × 100% (A.1) Where. Volume V --- titrate the sample consumed titanium trichloride standard titration solution, in milliliters (mL); C --- concentration of titanium trichloride standard titration solution, expressed in moles per liter (mol/L); Numerical m --- sample mass, in grams (g); M --- Carmine molar mass in grams per mole (g/mol), [M (C20H11N2Na3O10S3 · 1.5H2O) = 631.51]; 1000 --- volume conversion factor; 4 --- molar conversion factor. The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions Given absolute difference is not more than the arithmetic mean of 1.0%. A.4.2 Colorimetric method A.4.2.1 Method summary After dissolving each sample with a known water content Carmine reference, at the maximum absorption wavelength, were measured absorbance, then count Calculate its content. A.4.2.2 Reagents and materials A.4.2.2.1 ammonium acetate solution. 1.5g/L. A.4.2.2.2 Carmine reference. Content ≥85.0% (measured according to A.4.1). A.4.2.2.3 sulfuric acid solution. 120. A.4.2.3 instruments and equipment A.4.2.3.1 spectrophotometer. A.4.2.3.2 cuvette. 10mm. A.4.2.4 preparation of the reference solution carmine Weigh about 0.5g Carmine reference (accurate to 0.0001g), was dissolved in an appropriate amount of water, transferred to 1000mL volumetric flask, diluted with water To the mark. Imbibe 10mL, transferred to 500mL volumetric flask, add ammonium acetate solution was diluted to the mark, shake well and set aside. A.4.2.5 carmine aluminum lake preparation of the sample solution Weigh about 0.5g carmine aluminum lake sample (accurate to 0.0001g), was added sulfuric acid solution 20mL and 50mL freshly boiled and cooled To room temperature water, constantly shaking water bath heated to dissolve, transferred to 500mL volumetric flask, diluted with water to the mark. Draw 10mL, Transferred to 500mL volumetric flask, add ammonium acetate solution was diluted to the mark, shake, alternate (maximum absorption wavelength absorbance should be 0.3 to 0.7). A.4.2.6 analysis step The reference solution and carmine carmine aluminum lake sample solution were placed in 10mm cuvettes, with maximum absorption in the wavelength used Spectrophotometer respective absorbance values of ammonium acetate solution as reference solution. A.4.2.7 Calculation Results Carmine content mass fraction w1, according to equation (A.2) Calculated. w1 = A1 × m0 A0 × m1 × w0 × 2 × 100% (A.2) Where. A1 --- absorbance of the sample solution; Mass m0 --- carmine reference, in units of grams (g); A0 --- carmine reference absorbance of the solution; M1 --- the quality of the sample, in grams (g); Mass fraction,% (measured according to A.4.1) w0 --- carmine reference substance; 2 --- carmine aluminum lake standard solution and sample solution dilution. The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions Given absolute difference is not more than the arithmetic mean of 1.0%. A.5 Determination of hydrochloric acid insoluble matter A.5.1 Reagents and materials A.5.1.1 hydrochloric acid. A.5.1.2 hydrochloric acid solution. 5995. A.5.2 Instruments and Equipment A.5.2.1 crucible glass frit (G4). a pore size of 5μm ~ 15μm. A.5.2.2 oven thermostat. A.5.3 Analysis step Weigh about 5g sample (accurate to 0.001g), placed in 500mL beaker, add 250mL of water and 60mL of hydrochloric acid, cover the surface of the dish After heated to boiling, until the lake is completely dissolved. After cooling, it has 135 ℃ ± 2 ℃ drying to constant glass sand core crucible (G4) filter, and Using heated to 50 ℃ ~ 70 ℃ hot hydrochloric acid solution and the beaker was washed with a sintered glass crucible (the G4), until the washings were colorless, and then at 135 ℃ ± 2 ℃ constant temperature oven drying to constant weight. A.5.4 Calculation Results The mass fraction of hydrochloric acid insolubles w2, according to equation (A.3) Calculated. w2 = m2-m3 m4 × 100% (A.3) Where. m2 --- After drying quality hydrochloric acid insoluble matter and sand core glass crucible, in grams (g); M3 --- quality glass sand core crucible in grams (g); m4 --- sample mass, in grams (g). The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions Given absolute difference is not more than 0.2% of the arithmetic mean.

Appendix B

The method of preparation of titanium trichloride standard titration solution B.1 Reagents and materials B.1.1 hydrochloric acid. B.1.2 ferrous ammonium sulfate. B.1.3 ammonium thiocyanate solution.200g/L. B.1.4 sulfuric acid solution. 11. B.1.5 titanium trichloride solution. B.1.6 potassium dichromate standard titration solution. c 16K2Cr2O7 ÷ = 0.1mol/L. B.2 instruments and equipment Titration apparatus is shown in Figure A.1. Formulated B.3 titanium trichloride standard titration solution B.3.1 preparation Take appropriate amount of titanium trichloride solution and 75mL of hydrochloric acid placed 1000mL brown volumetric flask with freshly boiled and cooled to room temperature water Diluted to the mark, shake, immediately poured into a dark bottle under the mouth, stored under carbon dioxide gas. B.3.2 Calibration Weigh about 3g (accurate to 0.0001g) ferrous ammonium sulfate, 500mL Erlenmeyer flask placed under protective effect of carbon dioxide gas flow, plus Into 50mL freshly boiled and cooled water to dissolve, then add 25mL sulfuric acid was added, and the carbon dioxide stream fed subsurface for Protection, quickly and accurately added 35mL potassium dichromate standard titration solution, and then to be calibrated titanium trichloride standard solution titration to near meter Count the amount of the end, immediately added 25mL solution of ammonium thiocyanate, and continue to be calibrated with a standard solution of titanium trichloride titration to red to green Color, is the end. Entire titration should be under the protection of carbon dioxide gas flow operations, while doing the blank test. B.3.3 Calculation Results Titanium trichloride standard solution with a concentration per liter (mol/L) meter, according to equation (B.1) Calculated. c (TiCl3) = V × c V1-V2 (B.1) Where. Volume V --- potassium dichromate standard titration solution, in milliliters (mL); Concentration c --- Potassium dichromate standard titration solution, expressed in moles per liter (mol/L); V1 --- titration volume has been oxidized to potassium dichromate standard titration solution of titanium trichloride standard titration solution of the high titanium elapsed, the unit is Milliliter (mL of); V2 --- blank titration volume of spent titanium trichloride standard titration solution, in milliliters (mL). The results indicate four decimal. Calibration Calibration should immediately above in the analysis of samples.

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