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GB 1903.8-2015 English PDF

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GB 1903.8-2015: National Food Safety Standard -- Food Nutrition Enhancer -- Copper Gluconate
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Basic data

Standard ID GB 1903.8-2015 (GB1903.8-2015)
Description (Translated English) National Food Safety Standard -- Food Nutrition Enhancer -- Copper Gluconate
Sector / Industry National Standard
Classification of Chinese Standard X40
Word Count Estimation 9,939
Date of Issue 2015-11-13
Date of Implementation 2016-05-13
Regulation (derived from) National Health and Family Planning Commission Announcement No
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China

GB 1903.8-2015: National Food Safety Standard -- Food Nutrition Enhancer -- Copper Gluconate

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(National food safety standards of food nutrition fortifier copper gluconate) National Standards of People's Republic of China National Food Safety Standard Food fortifier copper gluconate Issued on. 2015-11-13 2016-05-13 implementation People's Republic of China National Health and Family Planning Commission released National Food Safety Standard Food fortifier copper gluconate

1 Scope

This standard applies to the copper gluconate or gluconate and copper oxidation reaction, crystallization derived food nutrition fortifier glucose Acid Copper Products; The product can also be glucose to gluconic acid after electrolysis with copper carbonate and made. 2 molecular formula, relative molecular mass and structural formula Formula 2.1 C12H22CuO14 2.2 formula 2.3 relative molecular mass 453.84 (according to 2011 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 Light blue color State fine powder Take the right amount of sample is placed in a clean, dry white porcelain plate , 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 Copper gluconate (to C12H22CuO14 dollars), w /% 98.0 ~ 102.0 Appendix A A.4 Reducing substances (with D-C6H12O6 meter), w /% ≤ 1.0 A.5 in Appendix A Total arsenic (As)/(mg/kg) ≤ 3.0 Appendix A A.6 Lead (Pb)/(mg/kg) ≤ 2.0 Appendix A A.7 Chloride (Cl dollars), w /% ≤ 0.07 Appendix A A.8 Sulfate (SO4 dollars), w /% ≤ 0.05 A.9 in Appendix A

Appendix A

Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive in accordance with the relevant provisions need to be careful when using the operation. If the Splashed on the skin should immediately wash with water, severe cases should be treated immediately. When using a volatile acid, it should be carried out in a fume hood. A.2 General Provisions Unless otherwise indicated in the analysis using only confirm three water as analytical reagent and GB/T 6682 stipulated. Test Methods Standard titration solution, impurities measured by standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601, GB/T 602, the provisions of the preparation of GB/T 603's. The solution in a solvent which does not indicate by when formulated, refers to an aqueous solution. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 hydrochloric acid. A.3.1.2 aqueous ammonia solution (6mol/L). Take a concentration of 28% ammonium hydroxide solution 400mL, diluted with water to 1000mL. The ammonia solution Content of 9.5% to 10.5%. A.3.1.3 potassium ferrocyanide solution (0.1g/mL). Weigh 1g potassium ferrocyanide [K4Fe (CN) 6 · 3H2O], was dissolved in 10mL water in. The solution is using now. A.3.1.4 acetic acid. A.3.1.5 phenylhydrazine. distilled before use. A.3.1.6 iron. Bright not rust. A.3.2 Identification method A.3.2.1 copper ions (Cu2) Identification A.3.2.1.1 sample solution Weigh 5.0g sample was dissolved in water and dilute to 100mL. A.3.2.1.2 analysis step A.3.2.1.2.1 proper amount of sample solution, adding a small amount of hydrochloric acid, into the piece of iron, iron sheet surface quickly form a red metallic copper film. A.3.2.1.2.2 proper amount of sample solution, the addition of excess ammonia solution, blue precipitate is generated, and then the precipitate was dissolved, the solution turns dark blue. A.3.2.1.2.3 take appropriate sample solution was added a solution of potassium ferrocyanide generated red-brown precipitate, the precipitate is insoluble in dilute nitric acid. A.3.2.2 Identification gluconate A.3.2.2.1 Method summary Samples in acetic acid medium, and phenylhydrazine were hot, a yellow crystalline glucose acid phenylhydrazine. A.3.2.2.2 Test Procedure Weigh copper gluconate sample 1.0g, dissolved in warm water, set the volume to 10mL, as the test solution. Take the test solution 5mL, was added 0.7mL 1mL of glacial acetic acid and phenylhydrazine, in a water bath heated 30min, to room temperature, the inner wall of the tube with a glass rod friction, the precipitated yellow crystals. A.3.2.3 Infrared Absorption Spectroscopy Using potassium bromide tablet method, tested in accordance with the provisions of GB/T 6040, and infrared spectra of the sample should be the control spectrum (spectrum control See Appendix B) consistent. A.4 copper gluconate (to C12H22CuO14 meter) measurement A.4.1 Method summary Under acidic conditions, the sample was added an excess of potassium iodide and cupric RQ, using starch as indicator, with sodium thiosulfate Precipitation titration standard solution of iodine. A.4.2 Reagents and materials A.4.2.1 potassium iodide. A.4.2.2 acetic acid. A.4.2.3 ammonium thiocyanate. A.4.2.4 sodium thiosulfate standard solution. c (Na2S2O3) = 0.1mol/L. A.4.2.5 starch indicator solution. 10g/L. A.4.3 Analysis step Weigh about 1.5g sample in 250mL Erlenmeyer flask (accurate to 0.001g), was added 100mL of water, and dissolved. Add 2mL of acetic acid And 5g potassium iodide and mix thoroughly. Titrated with standard sodium thiosulfate solution to a pale yellow. Add 2.0g of ammonium thiocyanate, mix, plus 3mL Starch indicator solution and continue titration to white. While doing the blank test. A.4.4 Calculation Results Copper gluconate mass fraction w1, expressed in%, according to equation (A.1) Calculated. w1 = (V-V0) × c × M m1 × 1000 × 100% (A.1) Where. Volume V --- titrate the sample solution consumption of sodium thiosulfate standard solution, in milliliters (mL); Volume V0 blank solution --- titration sample consumption of sodium thiosulfate standard solution, in milliliters (mL); c --- sodium thiosulfate standard solution concentration, in units of moles per liter (mol/L); Molar mass M --- copper gluconate, in units of grams per mole (g/mol), [M (C12H22CuO14) = 453.84]; M1 --- the quality of the sample, in grams (g); 1000 --- conversion factor. Independent determination results of two test results obtained under the repeatability condition of absolute difference is not more than 0.2%. A.5 Determination of reducing substances (with D-C6H12O6 basis) A.5.1 Method summary Under boiling conditions, reducing substances and excess copper gluconate or alkaline copper citrate solution produced by the reaction equivalent amount of cuprous oxide The precipitate was cooled. Hydrochloric acid was added to dissolve the cuprous precipitate was accurately added in excess iodine standard solution. Copper ions and a considerable amount of iodine occurs Redox reaction, excess iodine with sodium thiosulfate standard solution titration. By calculating the iodine consumption of copper ions, to calculate the sample Content of reducing substances. A.5.2 Reagents and materials A.5.2.1 alkaline copper citrate solution Weigh 173g sodium citrate (C6H5Na3O7 · 2H2O) and 117g of sodium carbonate (Na2CO3 · H2O), adding about 700mL water plus Heat to dissolve, filtered through a filter paper, if necessary. Weigh 17.3g of copper sulfate (CuSO4 · 5H2O) in another beaker, dissolved in water with about 100mL Was slowly added to the solution, was added during stirring constantly cooled, add water to 1000mL, and mix. A.5.2.2 iodine standard solution. c (12I2) = 0.1mol/L. A.5.2.3 sodium thiosulfate standard solution. c (Na2S2O3) = 0.1mol/L. A.5.2.4 starch indicator solution. 10g/L. A.5.2.5 acetic acid solution. 0.6mol/L. A.5.2.6 hydrochloric acid solution. 3mol/L. A.5.3 Analysis step Weigh about 1g sample in 250mL iodine flask (accurate to 0.001g), was dissolved in 10mL water. Alkaline Ning added 25.0mL Citric acid copper solution (A.5.2.1), in a small bottle covered with a watch glass and accurate micro-boiling 5min, rapidly cooled to room temperature. In acetic acid was added 25.0mL Solution (A.5.2.5), shake and accurately added 10.0mL of iodine standard solution (A.5.2.2), stopper tightly, shake, place 10min. Added 10mL Hydrochloric acid solution, then add starch indicator solution 3.0mL (A.5.2.4), immediately with sodium thiosulfate standard solution (A.5.2.3) titrated to the end point. A.5.4 Calculation Results Reducing substances (with D-C6H12O6 meter) mass fraction w2, expressed in%, according to equation (A.2) Calculated. w2 = (V1c1-V2c2) × 27 m2 × 1000 × 100% (A.2) Where. V1 --- exact volume addition of iodine standard solution, in milliliters (mL); c1 --- concentration of iodine standard solution, unit mole per liter (mol/L); Volume V2 --- titrate the sample solution consumed by sodium thiosulfate standard solution, in milliliters (mL); Concentration c2 --- sodium thiosulfate standard solution, the unit is mol per liter (mol/L); 27 --- empirically determined conversion factor for D- glucose units of grams per mole (g/mol); m2 --- sample mass, in grams (g); 1000 --- conversion factor. A.6 Determination of total arsenic (As) a (hydride generation atomic fluorescence spectrometry) Weigh about 0.5g sample in a beaker (to the nearest 0.001 g of), add water to dissolve 10mL, transferred to a 25mL volumetric flask, then added conc. Hydrochloric acid 1.25mL, water to the mark and shake. Take the above solution 10.0mL, set 100mL flask, add 50g/L thiourea solution Liquid 10mL, shaking constantly until a white precipitate is completely dissolved, with 5.0% hydrochloric acid solution (volume fraction) to the mark, shake, as the sample solution liquid. Following the second method according to GB 5009.76. A.7 Lead (Pb) Determination A.7.1 Graphite Furnace Atomic Absorption Spectrometry Weigh about 0.25g sample in 25mL volumetric flask (accurate to 0.001g), was added 15mL of water and dissolved by adding 2 drops of ultrasound concentrated nitric Acid, to the mark, as the sample solution. Following the first method according to GB 5009.12. A.7.2 Colorimetric The first method according to GB 5009.75 Determination. The method for processing a sample. Weigh about 5g sample into a beaker (accurate to 0.01g), plus After 10mL dissolved in water, dilute to 50mL. Were taken 10mL sample solution and 5.0mL of lead standard solution (lead content 0.005mg) in Two 125mL separating funnel, add water 10mL and 15mL. A.8 chloride (Cl) Determination A.8.1 Reagents and materials A.8.1.1 nitrate. A.8.1.2 silver nitrate solution. 0.10mol/L. A.8.1.3 chloride (Cl) standard solution. 0.02mol/L. A.8.2 Analysis step Weigh about 1g sample in 50mL colorimetric tube (accurate to 0.1g), add water to dissolve 30mL ~ 40mL. Were added 1mL Glass Acid, 1mL silver nitrate solution, dilute to 50mL, and mix. As a sample solution, and placing no direct sunlight 5min. Take 1.0mL chloride (Cl) standard solution in 50mL colorimetric tube, add 1mL of nitric acid, 1mL silver nitrate solution, the volume to 50mL, as a standard solution liquid. Turbidity of the sample solution can not be deeper than the turbidity standard solution, namely chloride content is less than or equal to 0.07%. A.9 Sulfate (SO4 meter) measurement A.9.1 Reagents and materials A.9.1.1 hydrochloric acid solution. 3mol/L. A.9.1.2 barium chloride solution. take 12g of barium chloride, dissolved in 100mL of water. A.9.1.3 Sulfate (SO4 meter) standard solution. 0.01mol/L. A.9.2 Analysis step Weigh about 2g sample in 50mL colorimetric tube (accurate to 0.1g), add water to dissolve 30mL ~ 40mL. Salt were added 1mL Acid solution, 3mL barium chloride solution, dilute to 50mL, and mix. Place 10min, as the sample solution. Take 1.0mL Sulfate ( SO4 meter) standard solution in 50mL colorimetric tube, hydrochloric acid solution is added 1mL, 3mL barium chloride solution, dilute to 50mL, mix, Place 10min, as a standard solution. Turbidity of the sample solution can not be deeper than the turbidity standard solution for less than or equal to 0.05% sulfate.

Appendix B

IR spectra of copper gluconate Copper gluconate infrared spectrum is shown in Figure B.1. Figure B.1 copper gluconate infrared spectrum NOTE. copper gluconate reference material from J

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