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GB 1886.220-2016 English PDF

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GB 1886.220-2016: Food additive Ponceau 4R
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GB 1886.220-2016English379 Add to Cart 3 days [Need to translate] Food additive Ponceau 4R Valid GB 1886.220-2016

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Basic data

Standard ID GB 1886.220-2016 (GB1886.220-2016)
Description (Translated English) Food additive Ponceau 4R
Sector / Industry National Standard
Classification of Chinese Standard X42
Word Count Estimation 19,147
Date of Issue 2016-08-31
Date of Implementation 2017-01-01
Older Standard (superseded by this standard) GB 4480.1-2001
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 1886.220-2016: Food additive Ponceau 4R

---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.
(Food safety national standard - Food additive - Carmine) National Standards of People's Republic of China National Food Safety Standard Carmine Food Additives 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 4480.1-2001 "food additive Carmine." This standard compared with GB 4480.1-2001, the main changes are as follows. --- Standard name was changed to "national food safety standards for food additives Carmine"; --- Modify the scope; --- Increasing the chemical name; --- Index name Appearance modify sensory requirements; --- Loss on drying and chloride (based on NaCl) and sulfate (Na2SO4 to count) aggregates merger; --- Increasing the unreacted intermediate sum, non-sulfonated aromatic primary amine (aniline dollars) index requirements and test methods; --- Heavy Metals (as Pb) Index name changed to lead, to modify the test method; --- Revised test methods for arsenic; --- Modify the authentication method. National Food Safety Standard Carmine Food Additives

1 Scope

This standard applies to post-1- naphthylamine 4-sulfonate as raw material by diazotization of 2-naphthol-6,8-disulfonic acid, potassium coupled prepared food Carmine additive. 2 chemical name, molecular formula, molecular mass and structural formula 2.1 Chemical Name 1- (4'-sulfo-1'-naphthyl) azo-2-naphthol-6,8-disulfonic acid trisodium salt Formula 2.2 C20H11N2Na3O10S3 · 1.5H2O 2.3 formula 2.4 relative molecular mass 631.51 (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 Color red to dark red The state of a powder or granules 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, w /% ≥ 85.0 Appendix A A.4 Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 to count) Total, w /% ≤ 18.0 Appendix A A.5 Water-insoluble, w /% ≤ 0.20 A.6 in Appendix A Deputy dye, w /% ≤ 3.0 Appendix A A.7 Unreacted intermediate sum, w /% ≤ 0.5 Appendix A A.8 Unsulfonated primary aromatic amine (aniline dollars), w /% ≤ 0.01 A.9 in Appendix A Arsenic (As)/(mg/kg) ≤ 1.0 GB 5009.11 or GB 5009.76 Lead (Pb)/(mg/kg) ≤ 10.0 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 Ammonium acetate solution. 1.5g/L. A.3.2 Instruments and Equipment A.3.2.1 Spectrophotometer. A.3.2.2 cuvette. 10mm. A.3.3 Identification method A.3.3.1 dissolution test Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL of water was red clear solution. A.3.3.2 Test absorbance Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL ammonium acetate solution of this solution 1mL, plus ammonium acetate solution equipped to 100mL, the maximum absorption wavelength of this solution is 505nm ~ 510nm. Note. The measured absorbance value should be 0.3 to 0.7, otherwise adjust the concentration of the sample. A.4 Determination of the content of carmine A.4.1 Titanium trichloride titration (Arbitration Act) A.4.1.1 Method summary In alkaline 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 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 0.5g sample (accurate to 0.0001g), placed in 500mL conical flask, dissolved in 50mL freshly boiled and cooled to room temperature Water, adding 15g trisodium citrate and 150mL of freshly boiled water, dissolved by shaking, according to Figure A.1 instrument installed at the surface through dioxide Carbon while heating to a boil, and treated with titanium trichloride standard titration solution to titrate the sample solution inherent color disappears 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. V --- titration sample consumed titanium trichloride standard titration solution volume in milliliters (mL); c --- titanium trichloride standard titration solution concentration, in units of moles per liter (mol/L); M --- Carmine molar mass in grams per mole (g/mol) [M (C20H11N2Na3O10S3 · 1.5H2O) = 631.51]; M --- the quality of the sample, in grams (g); 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.4.2.3 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, spare (maximum Absorbance at a wavelength of absorption should be 0.3 to 0.7). Preparation of the sample solution A.4.2.5 carmine Weighing and methods of operation with carmine preparation of the reference solution. A.4.2.6 analysis step The carmine carmine sample solution and reference solution were placed in 10mm cuvettes, with the maximum absorption wavelength using a spectrophotometer Meter measuring their absorbance 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 × 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 w0 --- Carmine reference standard (measured according to A.4.1),%. 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 loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) of the total A.5.1 Determination of loss on drying A.5.1.1 Method summary Sample is placed in a weighing bottle and dried in a thermostatic oven to constant mass after weighing the material after drying. A.5.1.2 instruments and equipment Ovens. A.5.1.3 analysis step Weigh about 2g sample (accurate to 0.0001g), has placed constant at 135 ℃ ± 2 ℃ constant temperature oven φ (30 ~ 40) mm, said Flask, at 135 ℃ ± 2 ℃ constant temperature oven drying to constant weight. A.5.1.4 Calculation Results Loss on drying mass fraction w2, according to equation (A.3) Calculated. w2 = m2-m3 m4 × 100% (A.3) Where. M2 --- sample mass before drying and weighing bottles in grams (g); m3 --- After drying to constant mass and weighing the sample bottles 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. A.5.2 chloride (as NaCl) Determination A.5.2.1 Method summary An acidic medium a known amount of silver nitrate solution, the chlorine ion as silver chloride precipitate, ferric ammonium sulfate solution was then added as a Indicator, the use of ammonium thiocyanate standard titration solution titrate the excess silver nitrate. A.5.2.2 Reagents and materials A.5.2.2.1 nitrobenzene. A.5.2.2.2 nitric acid solution. 11. A.5.2.2.3 silver nitrate solution. c (AgNO3) = 0.1mol/L. A.5.2.2.4 ammonium ferric sulfate solution. Weigh 14g of ammonium ferric sulfate, dissolved in 100mL of water, filter, add 10mL of nitric acid, stored in brown Bottle. A.5.2.2.5 ammonium thiocyanate standard titration solution. c (NH4SCN) = 0.1mol/L. A.5.2.2.6 carbon. 767 needle. A.5.2.3 preparation of the sample solution Weigh about 2g sample (accurate to 0.0001g), was dissolved in 150mL of water, add about 15g of activated carbon, a moderate boil 2min ~ 3min. Cooled to room temperature, a solution of nitric acid was added 1mL, continue to shake evenly placed 30min (from time to time during the swing). Filtered through a dry filter paper. Such as The filtrate was colored, then coupled with activated carbon 5g, placed 60min (during shaking from time to time), and then dried filter paper (such as color still replace the activated carbon Repeat until the filtrate was colorless). 10mL each wash with water three times activated carbon, and the filtrate combined move 200mL volumetric flask, add water to the mark, Shake well. For the determination of chloride and sulfate content. A.5.2.4 analysis step Pipette 50mL sample solution, placed in 500mL conical flask, add 10mL 2mL nitric acid solution and silver nitrate solution (chloride more May be appropriate to pay more) and 5mL nitrobenzene, shake vigorously to silver chloride coagulation, ferric ammonium sulfate is added 1mL solution, with drops of ammonium thiocyanate standard Given titrate the excess silver nitrate to the end and keep 1min, at the same time in the same way blank test. A.5.2.5 Calculation Results Chloride (as NaCl) mass fraction w3, according to equation (A.4) Calculated. w3 = V1-V0 1000 × c1 × M1 m5 × × 100% (A.4) Where. V1 --- blank titration solution consumed volume of ammonium thiocyanate standard titration solution, in milliliters (mL); V0 --- titration sample consumption volume of ammonium thiocyanate standard titration solution, in milliliters (mL); 1000 --- volume conversion factor; c1 --- ammonium thiocyanate standard titration solution concentration, in units of moles per liter (mol/L); --- Ml molar mass of sodium chloride, in units of grams per mole (g/mol) [M (NaCl) = 58.4]; M5 --- the quality of the sample, in grams (g); Volume 50 --- Pipette sample solution, in milliliters (mL); 200 --- dose volume of sample solution, in milliliters (mL). The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions Given the absolute difference between the results of not more than 0.3% of the arithmetic mean. A.5.3 Sulfate (Na2SO4 meter) measurement A.5.3.1 Method summary The sample solution of barium chloride standard titration solution, barium sulfate ion to form sulfate precipitation, with rose red indicator solution of sodium as an external means It shows agents used to determine the titration end point. A.5.3.2 Reagents and materials A.5.3.2.1 sodium hydroxide solution. 0.2g/L. A.5.3.2.2 hydrochloric acid solution. 11999. A.5.3.2.3 barium chloride standard titration solution. c 12BaCl2 ÷ = 0.1mol/L (preparation see Appendix C). A.5.3.2.4 phenolphthalein indicator solution. 10g/L. A.5.3.2.5 Rose sodium indicator solution. Weigh 0.1g of sodium red roses, was dissolved in 10mL of water (using now). A.5.3.3 analysis step Draw 25mL sample solution (A.5.2.3), placed in 250mL conical flask, add 1 drop of phenolphthalein indicator solution, sodium hydroxide solution was added dropwise Pink, then a solution of hydrochloric acid solution to the pink color disappeared, shake, titrated with barium chloride standard titration solution is constantly shaking dissolved, with rose Rose red indicator solution of sodium for outward indicator solution, and the reaction liquid indicator solution on filter paper presents the intersection of rose red spots and kept 2min does not fade As the end point. At the same time in the same manner as a blank test. A.5.3.4 Calculation Results Sulfate (Na2SO4 meter) mass fraction w4, according to equation (A.5) Calculated. w4 = V3-V2 1000 × c2 × M2 m6 × × 100% (A.5) Where. Volume V3 --- titration solution consumed barium chloride standard titration solution, in milliliters (mL); V2 --- blank titration solution consumed volume of barium chloride standard titration solution, in milliliters (mL); 1000 --- volume conversion factor; c2 --- barium chloride standard titration solution concentration, in units of moles per liter (mol/L); Molar mass of the M2 --- sodium sulfate, units of grams per mole (g/mol) [M (Na2SO4) = 142]; 2 --- molar conversion factor; M6 --- the quality of the sample, in grams (g); Volume 25 --- pipetting the sample solution, in milliliters (mL); 200 --- dose volume of sample solution, in milliliters (mL). 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. Results A.5.4 Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) the total amount of calculation Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) of the total mass fraction w5, according to equation (A.6) Calculated. w5 = w2 w3 w4 (A.6) Where. w2 --- Loss on drying mass fraction,%; w3 --- chloride (as NaCl) mass fraction,%; w4 --- Sulfate (Na2SO4 meter) mass fraction,%. The results represent a decimal. A.6 Determination of insoluble matter A.6.1 Method summary After the sample was dissolved filtration, placed in a thermostatic oven dried to constant mass after weighing the insoluble material. A.6.2 Instruments and Equipment A.6.2.1 crucible glass frit (G4). a pore size of 5μm ~ 15μm. A.6.2.2 oven thermostat. A.6.3 Analysis step Weigh about 3g sample (accurate to 0.001g), placed in 500mL beaker, add 50 ℃ ~ 60 ℃ water 250mL, dissolved, (G4) filter has been used in 135 ℃ ± 2 ℃ drying to constant sand core glass crucible and washed thoroughly with hot water to the washing liquid colorless, ± at 135 ℃ 2 ℃ constant temperature oven drying to constant weight. A.6.4 Calculation Results The mass fraction of water-insoluble w6, according to equation (A.7) calculated as follows. w6 = m7-m8 m9 × 100% (A.7) Where. m7 --- After drying quality water insoluble and glass sand core crucible in grams (g); M8 --- quality glass sand core crucible in grams (g); m9 --- sample mass, in grams (g). The results parallel arithmetic mean of the measurement results shall prevail (2 decimal places). In two independent test repeated conditions Given absolute difference is not more than 0.2% of the arithmetic mean. Determination A.7 deputy dye A.7.1 Method summary The components are separated by paper chromatography, eluted and quantified by spectrophotometry. A.7.2 Reagents and materials A.7.2.1 ethanol. A.7.2.2 n-butanol. Acetone solution A.7.2.3. 1 1. A.7.2.4 ammonia solution. 496. A.7.2.5 sodium bicarbonate solution. 4g/L. A.7.3 Instruments and Equipment A.7.3.1 Spectrophotometer. A.7.3.2 chromatography filter paper. No. 1 in speed, 150mm × 250mm. A.7.3.3 chromatography tank. φ240mm × 300mm. A.7.3.4 micro injector. 100μL. A.7.3.5 Nessler colorimetric tube. 50mL glass grinding mouth stopper. A.7.3.6 glass frit funnel (G3). a pore diameter of 15μm ~ 40μm. A.7.3.7 50mm cuvette. A.7.3.8 10mm cuvette. A.7.4 Analysis step A.7.4.1 paper chromatographic conditions A.7.4.1.1 developing solvent. n-butanol ethanol solution of aqueous ammonia = 623. A.7.4.1.2 Temperature. 20 ℃ ~ 25 ℃. A.7.4.2 preparation of the sample solution Weigh about 1g sample (accurate to 0.001g), placed in a beaker, adding the right amount of water dissolved and transferred to 100mL volumetric flask, dilute to Scale, shake up the concentration of the sample solution is 1%. A.7.4.3 wash out the sample preparation liquid With micro-injector draw 100μL sample solution evenly note on the bottom edge of the filter paper from a baseline of 25mm, a straight line, so that On filter paper width is not more than 5mm, length 130mm, with a hair dryer. The filter paper containing preformulated good developer Expand the chromatography tank, filter paper dipped under the bottom edge of the agent level 10mm, to be solvent front line rose to 150mm or until the dye deputy Separation satisfied. Remove the filter paper chromatography, with cold dry. Blank filter paper under the same conditions to expand the blank paper and the above steps should be expanded with the adjacent portion of the filter paper on the same piece of filter paper Clipping. Deputy dye paper chromatography is shown in Figure A.2. Figure A.2 deputy dye paper chromatography schematic After each sub-dye made and will start on a blank paper to each subsidiary colors corresponding parts of the paper in the same size cut, and Cut into thin strips about 5mm × 15mm, and were placed in 50mL of Nessler colorimetric tube, accurately added to the acetone solution 5mL, shake 3min ~ 5min, then the exact solution of sodium bicarbonate was added 20mL, shake well, and then were in the glass frit funnel (G3) in natural filtration, filtration Liquid should be clarified without suspension. Respectively each subsidiary colors and blank eluate. Deputy dye in their maximum absorption wavelength, with 50mm cuvette, wash the dye out of each sub-liquid measuring their absorbance on a spectrophotometer. When the absorbance was measured on a spectrophotometer, with a mixture of 5mL and 20mL acetone solution of sodium bicarbonate solution as a reference solution. A.7.4.4 preparation of standard solution 2mL1% of the sample solution is transferred to absorb 100mL volumetric flask, dilute to the mark, shake, and the solution as the standard solution. A.7.4.5 Preparation of standard eluate With micro-injector draw 100μL standard solution, uniform injection site on the bottom edge of the filter paper from a baseline of 25mm with a hair dryer blowing dry. The filter paper containing previously prepared well eluent chromatography tank to expand, to be solvent front line up 40mm, remove with cold wind Dry, cut out all the dye partially deployed, according to A.7.4.3 operating procedure, the standard eluate. 10mm cuvette with maximum suction Absorbance was measured at a wavelength of income. Meanwhile blank filter paper under the same conditions to start operating in the same manner after the measured absorbance white wash liquid. A.7.4.6 Calculation Results Mass fraction deputy dye w7, according to equation (A.8) Calculated. w7 = Σ An-bn () As-bs () × × w1 × 100% (A.8) Where. An --- each sub-dye eluate 50mm optical path length measured absorbance; bn --- dye control each sub-blank eluate 50mm optical path length measured absorbance; 5 --- converted into multiples of 10mm optical path length; As --- Standard eluate 10mm path length measured absorbance; bs --- standard control blank eluate 10mm path length measured absorbance; --- Standard eluate converted into multiples of one percent of the sample solution; Mass fraction w1 --- sample,%. The results represent a decimal. 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. A.8 Determination of unreacted intermediate sum A.8.1 Method summary By reverse-phase liquid chromatography, using external standard method were not quantified the various reaction intermediates, the final calculation of the sum of the unreacted intermediate mass fraction. A.8.2 Reagents and materials A.8.2.1 methanol. A.8.2.2 ammonium acetate solution. 0.02mol/L. A.8.2.3 1- naphthylamine 4-sulfonate. A.8.2.4 7- hydroxy-1,3-naphthalene sulfonate. A.8.2.5 3- hydroxy-2,7-naphthalene sulfonate. A.8.2.6 6- hydroxy-2-naphthalene sulfonate. A.8.3 Instrum...

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