GB 4479.1-2010 English PDFUS$489.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 4479.1-2010: Amaranth national food safety standards of food additives Status: Valid GB 4479.1: Historical versions
Basic dataStandard ID: GB 4479.1-2010 (GB4479.1-2010)Description (Translated English): Amaranth national food safety standards of food additives Sector / Industry: National Standard Classification of Chinese Standard: X42 Classification of International Standard: 67.220.20 Word Count Estimation: 21,278 Date of Issue: 2010-12-21 Date of Implementation: 2011-02-21 Older Standard (superseded by this standard): GB 4479.1-1999 Regulation (derived from): Ministry of Health Bulletin No. 19 of 2010 Issuing agency(ies): Ministry of Health of the People's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 for 1 naphthylamine -4 sulfonate by diazotization with a 2 naphthol -3 disulfonate coupling obtained food additives amaranth. GB 4479.1-2010: Amaranth national food safety standards of food additives---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.Amaranth national food safety standards of food additives National Food Safety Standard Food Additives Amaranth 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 ForewordThis standard replaces GB 4479.1-1999 "food additives amaranth." This standard compared with GB 4479.1-1999, the main changes are as follows. - Added safety tips; - Canceled ≥60.0% quality specifications; - Water insoluble ≤0.30% by the index revised to ≤0.20%; - Modify the discrimination test methods; - Colorimetric method allows parallel determination by the difference of 2.0% revised to 1.0%; - An increase of intermediate indicators and detection methods unreacted; - Added unsulfonated primary aromatic amine (aniline meter) indicators and detection methods; - Arsenic (As) is modified by chemical detection methods limit law atomic absorption spectrometry; - Cancel the heavy metals (Pb) quality specifications; - Increase the lead (Pb) indicator and detection methods. The Standard Appendix A, Appendix B and Appendix C are normative appendices, Appendix D is an informative annex. This standard replaces the standards previously issued as follows. --GB 4479.1-1986, GB 4479.1-1996, GB 4479.1-1999. National Food Safety Standard Food Additives Amaranth1 ScopeThis standard applies to 1-naphthylamine 4-sulfonate diazotization after with 2-naphthol-3,6-sodium coupling obtained food additives amaranth Red dish.2 Normative referencesThe standard file referenced in the application of this standard is essential. For cited documents with dates, only the date of Version applies to this standard. For undated references, the latest edition (including any amendments) applies to this standard. 3 chemical name, structural formula, molecular formula and relative molecular mass 3.1 Chemical Name 3-hydroxy-4- (4-azo-naphthalene sulfonic acid) 2,7-naphthalene disulfonic acid trisodium salt 3.2 Structure. Formula 3.3 C20H11N2Na3O10S3 3.4 relative molecular mass 604.48 (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 Red-brown to dark brown color By visual assessment of natural light. State organization powders or granules 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Amaranth, w /% ≥ 85.0 Appendix A A.4 Loss on drying, chloride (based on NaCl) and sulfate (NaSO4 in dollars) of the total, w /% ≤ 15.0 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 /% ≤ 0.50 Appendix A A.8 Unsulfonated primary aromatic amine (aniline dollars), w /% ≤ 0.01 A.9 in Appendix A Arsenic (As)/(mg/kg) ≤ 1.0 Appendix A A.10 Lead (Pb)/(mg/kg) ≤ 10.0 Appendix A A.11Appendix A(Normative) Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, according to the relevant provisions of the operation, the operation need to be careful. If splashed on the skin should immediately wash 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 This standard reagents and water, did not indicate when the other requirements, refer to three analytical reagent and GB/T 6682-2008 specified water. Standard test solution required impurity standard solution, preparations and products at the time did not indicate other provisions, according to GB/T 601, GB/T 602, GB/T 603 regulations formulated and calibration. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 sulfuric acid. A.3.1.2 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 It should meet the following conditions. A.3.3.1 Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL of water was red clear solution. A.3.3.2 Weigh about 0.2g sample (accurate to 0.01g), add 20mL sulfuric acid, the solution was purple, take this solution 2 drops to 3 drops of water was added 5mL The red color. A.3.3.3 Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL ammonium acetate solution of this solution 1mL, plus ammonium acetate solution Liquid distribution to 100mL, the maximum absorption wavelength of the solution was 520 nm ± 2nm. A.4 Determination of Amaranth A.4.1 Titanium trichloride titration (Arbitration Act) A.4.1.1 Method summary In acidic medium, amaranth 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 cylinders loaded carbon dioxide. A.4.1.3 instruments and equipment A-- conical flask (a 500 mL); B-- Brown burette (50mL); C-- under glass bottle package black paper (2000mL); D-- containing 100g/L solution of ammonium carbonate and 100g/L ferrous sulfate solution container of an equivalent mixture (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 Erlenmeyer flask was dissolved in 50mL boiling water and cooled to room temperature Added 15g trisodium citrate and 150mL boiled water, dissolved by shaking, according to Figure A.1 instrument installed at the surface through dioxide Carbon while heating boil, and treated with a solution of titanium trichloride standard titration titration end point so that the inherent color disappeared. A.4.1.5 Calculation Results Amaranth mass fraction 1w its value is expressed in%, according to formula (A.1) Calculated. 0) 4 /) (1000/( 1 × = m MVcw (A.1) Where. c - accurate titanium trichloride standard titration solution concentration value in units of moles per liter (mol/L); V - accurate value of the sample consumed titration of titanium trichloride standard titration solution volume in milliliters (mL); M - molar mass of Amaranth value, in units of grams per mole (g/mol) [M (C20H11N2Na3O10S3) = 604.48]; m1 - mass value of the sample in grams (g). The results represent a decimal. The absolute difference between the parallel determination results is not more than 1.0% (mass fraction), the arithmetic mean value as a measurement result. A.4.2 Colorimetric method A.4.2.1 Method summary The samples with known content of amaranth standards were dissolved in water and diluted to volume with ammonium acetate solution, the maximum absorption wavelength At its absorbance values were measured to 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 amaranth standard. ≥85.0% (mass fraction, 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. Preparation A.4.2.4 amaranth standard sample solution Weigh about 0.5g Amaranth standard (accurate to 0.0001g), was dissolved in an appropriate amount of water, transferred to 1000mL volumetric flask, dilute with water Release to the mark. Draw 10mL, transferred to 500mL volumetric flask, add ammonium acetate solution was diluted to the mark, shake well and set aside. Preparation A.4.2.5 amaranth sample solution A.4.2.4 weighing and methods of operation with standard solution preparation. A.4.2.6 analysis step The standard solution amaranth and amaranth sample solution were placed in 10mm cuvettes, with the maximum absorption wavelength using a spectrophotometer Meter measuring their absorbance values with ammonium acetate solution as the reference solution. A.4.2.7 Calculation Results Amaranth mass fraction 1w its value is expressed in%, according to formula (A.2) Calculated. 1 wmA Amw × = (A.2) Where. A - absorbance of amaranth sample solution value; Numerical m0-- amaranth standard mass in grams (g); Amaranth A0-- absorbance value of the standard solution; Sample quality m-- value in units of grams (g); w0-- amaranth standard mass fraction%. The results represent a decimal. The absolute difference between the parallel determination results is not more than 1.0% (mass fraction), the arithmetic mean value as a measurement result. A.5 Determination of loss on drying, chloride (based on NaCl) and sulfate (Na2S04 in dollars) of the total A.5.1 Determination of loss on drying A.5.1.1 analysis step Weigh about 2g sample (accurate to 0.001g), has been placed in the weighing bottle 135 ℃ ± 2 ℃ oven temperature constant at at 135 ℃ ± 2 ℃ constant temperature oven drying to constant weight. A.5.1.2 Calculation Results Loss on drying mass fraction to 2w and its value is expressed in%, according to formula (A.3) Calculated. 2 × - = m mmw (A.3) Where. Numerical m2-- sample before drying mass in grams (g); m3-- sample dried to a constant mass values, expressed in grams (g). The results represent a decimal. The absolute difference between the parallel determination results is not more than 0.2% (mass fraction), the arithmetic mean value as a measurement result. A.5.2 chloride (as NaCl) Determination A.5.2.1 Reagents and materials A.5.2.1.1 nitrobenzene. A.5.2.1.2 activated carbon; 767 needle. A.5.2.1.3 nitric acid solution. 11. A.5.2.1.4 silver nitrate solution. c (AgNO3) = 0.1mol/L. A.5.2.1.5 ammonium ferric sulfate solution. Preparation method. Weigh about 14g of ammonium ferric sulfate, dissolved in 100mL of water, filter, add 10mL of nitric acid, stored in a brown bottle. A.5.2.1.6 ammonium thiocyanate standard titration solution. c (NH4CNS) = 0.1mol/L. A.5.2.2 preparation of the sample solution Weigh about 2g sample (accurate to 0.001g), was dissolved in 150mL of water, add about 15g of activated carbon, a moderate boil 2 min ~ 3min, plus The nitric acid solution 1mL, continue to shake evenly placed 30min (during shaking from time to time). Filtered through a dry filter paper. Such as colored filtrate is then Add 5g of activated carbon, occasionally shaking place 1h, then dried filter paper (such as color still replace the activated carbon Repeat until the filtrate colorless). 10mL each wash with water three times activated carbon, and the filtrate combined move 200mL volumetric flask, add water to the mark. For chloride and sulfur Determination of salt content. A.5.2.3 analysis step Pipette 50mL sample solution, placed in 500mL conical flask, add 10mL 2mL nitric acid solution and silver nitrate solution (chloride content more To add more) and 5mL nitrobenzene, shake vigorously to silver chloride condensation, ammonium ferric sulfate is added 1mL solution with ammonium thiocyanate standard titration Titrate the excess silver nitrate to the end and keep 1min, at the same time in the same way to make a blank test. A.5.2.4 Calculation Results Chloride (as NaCl) mass fraction 3w and its value is expressed in%, according to formula (A.4) Calculated. ) 200/50 ( ] 1000 /) [( 3 × - = m MVVcw (A.4) Where. c1 - accurate ammonium thiocyanate standard titration solution concentration value in units of moles per liter (mol/L); V1 - accurate value of consumption of titration blank solution of ammonium thiocyanate standard titration solution volume in milliliters (mL); V0 - accurate value of the sample solution was titrated with ammonium thiocyanate standard titration solution consumed volume in milliliters (mL); M1 - the value of the molar mass of sodium chloride, in units of grams per mole (g/mol) [M1 (NaCl) = 58.4]; Sample quality m4-- value in units of grams (g). The results represent a decimal. Parallel determination results of absolute difference is not more than 0.3% (mass fraction), the arithmetic mean value as a measurement result. A.5.3 Sulfate (Na2S04 meter) measurement A.5.3.1 Reagents and materials A.5.3.1.1 sodium hydroxide solution. 2g/L. A.5.3.1.2 hydrochloric acid solution. 11999. A.5.3.1.3 barium chloride standard titration solution. c (1/2BaCl2) = 0.l mol/L (preparation see Appendix C). A.5.3.1.4 phenolphthalein indicator solution. 10g/L. A.5.3.1.5 Rose sodium indicator solution. Weigh 0.lg red roses, sodium dissolved in 10mL of water (using now). A.5.3.2 analysis step Draw 25mL sample solution (A.5.2.2), placed in 250mL conical flask, add 1 drop of phenolphthalein indicator solution, a solution of sodium hydroxide solution Pink, then a solution of hydrochloric acid solution to the pink color disappeared, shake, dissolved in constant shaking drops of barium chloride standard titration solution Set in red roses sodium indicator solution for outward indicator solution, and the reaction liquid indicator solution on filter paper presents the intersection of rose red spots and kept 2min Do not fade as the end point. At the same time in the same manner as a blank test. A.5.3.3 Calculation Results Sulfate (Na2SO4 meter) mass fraction 4w and its value is expressed in%, according to formula (A.5) Calculated. ) 200/25 ( ) 2 /] (1000 /) [( 4 × - = m MVVcw (A.5) Where. c2 - accurate barium chloride standard titration solution concentration value in units of moles per liter (mol/L); The exact value of the sample solution V2-- titration consumption of barium chloride standard titration solution volume in milliliters (mL); Accurate value of V3-- titrate blank solution consumed barium chloride standard titration solution volume in milliliters (mL); M2 - the value of the molar mass of sodium sulfate, units of grams per mole (g/mol) [M2 (Na2SO4) = 142.04]; m4 - mass of the sample value in units of grams (g). The results represent a decimal. The absolute difference between the parallel determination results is not more than 0.2% (mass fraction), the arithmetic mean value as a measurement result. Results A.5.4 Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) the total amount of calculation Total loss on drying and chloride (based on NaCl) and sulfate (Na2SO4 to count) to the mass fraction 5w and its value is expressed in% According to the formula (A.6) Calculated. 4325 wwww = (A.6) Where. 2w - drying loss mass fraction%; 3w - chloride (as NaCl) mass fraction%; 4w - Sulfate (Na2SO4 meter) mass fraction%. The results represent a decimal. A.6 Determination of insoluble matter A.6.1 Instruments and Equipment A.6.1.1 sand core glass crucible. G4, a pore size of 5μm ~ 15μm. A.6.1.2 oven thermostat. A.6.2 Analysis step Weigh about 3g sample (accurate to 0.001g), placed in 500mL beaker, add 50 ℃ ~ 60 ℃ hot water 250mL, dissolved, Has been used in 135 ℃ ± 2 ℃ drying to constant glass sand core crucible filtered and washed thoroughly with hot water to wash colorless liquid at 135 ℃ ± 2 ℃ Thermostatic oven drying to constant weight. A.6.3 Calculation Results Water insoluble mass fraction 6w and its value is expressed in%, according to formula (A.7) calculated as follows. 6 × = m mw (A.7) Where. m6 - Numerical dried water insoluble mass in grams (g); m5 - the value of the sample mass, in grams (g). The results represent two decimal. The absolute difference between parallel determination results is not more than 0.05% (mass fraction), the arithmetic mean value as a measurement result. 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, pore size 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 1g sample (accurate to 0.001g), placed in a beaker, after adding an appropriate amount of water dissolved and transferred to 100mL volumetric flask, dilute To the mark, shake up the concentration of the sample solution was 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, Its width on the filter paper does not exceed 5mm, length 130mm, with a hair dryer. The filter paper containing preformulated good Expand Chromatography tank agent, expand, filter paper dipped under the bottom edge of the agent level l0mm, to be solvent front line rose to 150mm or until the dye deputy Material separation satisfaction. 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. Baseline Main dye 130mm 150mm 250mm 25mm Vice-dye (4) Deputy Dye (3) Vice-dye (2) Deputy dye (1) Figure A.2 deputy dye paper chromatography schematic The respective deputy dye expanded and made 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 5mL acetone, shaking 3min ~ 5min, then the exact solution of sodium bicarbonate was added 20mL, shake well, and then were naturally filtered G3 sintered glass funnel, The filtrate 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 Draw a sample solution 6mL 1% moved into 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 to draw standard solution 100μL, uniform injection site on the bottom edge of the filter paper from a baseline of 25mm with a hair dryer Dry. The filter paper containing previously prepared well eluent chromatography tank to expand, to be solvent front line up 40mm, remove with cold Dry, cut out all the dye partially deployed, according to A.7.4.3 subjected to extraction methods to obtain standard eluate. Colorimetric with 10mm Dish at the maximum absorption wavelength measured absorbance values. Meanwhile blank filter paper under the same conditions to start operating in the same manner after washing the absorbance value measured liquid. 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