GB 1886.37-2015 English PDF

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GB 1886.37-2015: National Food Safety Standard -- Food Additives -- Sodium cyclamate
Status: Valid

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Basic data

Standard ID: GB 1886.37-2015 (GB1886.37-2015)
Description (Translated English): National Food Safety Standard -- Food Additives -- Sodium cyclamate
Sector / Industry: National Standard
Classification of Chinese Standard: X42
Classification of International Standard: 67.220.20
Word Count Estimation: 11,150
Date of Issue: 2015-09-22
Date of Implementation: 2016-03-22
Older Standard (superseded by this standard): GB 12488-2008
Regulation (derived from): PRC National Health and Family Planning Commission 2015 No.8
Issuing agency(ies): National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 1886.37-2015: National Food Safety Standard -- Food Additives -- Sodium cyclamate

---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.
(National food safety standards for food additives aminocyclohexylamino sulfonate (aka sodium cyclamate)) National Standards of People's Republic of China National Food Safety Standard Food additives cyclohexylamino sulfonate (Also known as sodium cyclamate) Issued on. 2015-09-22 2016-03-22 implementation People's Republic of China National Health and Family Planning Commission released

Foreword

This standard replaces GB 12488-2008 "Food Additives cyclamic sodium (sodium cyclamate)." This standard compared with GB 12488-2008, the main changes are as follows. --- Standard name was changed to "national food safety standards for food additives cyclohexylamino sodium (also known as sodium cyclamate)." National Food Safety Standard Food additives cyclohexylamino sulfonate (Also known as sodium cyclamate)

1 Scope

This standard applies to glucose as raw materials by fermentation, esterification, conversion, refining prepared food additive cyclohexylamino sodium (aka Cyclamate). 2 chemical name, molecular formula, molecular mass and structural formula 2.1 Chemical Name Cyclohexylamino sulfonate. Formula 2.2 C6H12NNaO3S · nH2O (anhydrous product n = 0, the crystals of n = 2) 2.3 formula 2.4 relative molecular mass Dry goods 201.22; crystalline product 237.25 (according to 2007 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 Claim Anhydrous crystalline products product Testing method Color White State white crystalline powder, needle-like crystal white needles, lamellae Odour odorless Take the right amount of sample is placed in a clean, dry white porcelain dish, natural Light, color and observe the state of its taste and olfactory 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 project index Anhydrous crystalline products product Testing method Cyclohexylamino sodium content (dry basis), w /% ≥ 98.0 ~ 101.0 Appendix A A.4 Sulfate (SO4 dollars), w /% ≤ 0.10 Appendix A A.5 pH (100g/L aqueous solution) 5.5 to 7.5 Appendix A A.6 Loss on drying, w /% ≤ 0.5 16.5 Appendix A A.7 Amino acid, w /% ≤ 0.15 Appendix A A.8 Cyclohexylamine, w /% ≤ 0.0025 A.9 in Appendix A Dicyclohexylamine by test A.10 in Appendix A Absorbance (100g/L solution) ≤ 0.10 Appendix A A.11 Transparency (expressed as transmittance 100g/L solution) /% ≥ 95.0 Appendix A A.12 Heavy metals (Pb)/(mg/kg) ≤ 10.0 Appendix A A.13 Arsenic (As)/(mg/kg) ≤ 1.0 GB 5009.76

Appendix A

Testing method A.1 Warning Reagents The standard test methods used for toxic or corrosive, care should be taken. As splashed on the skin should stand That is rinsed with water, severe cases should be treated immediately. When using the virulent, should be strictly in accordance with the relevant provisions of the management; should be used to avoid inhalation or skin Skin contact should be necessary in a fume hood. 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 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 ether. A.3.1.2 nitrate. A.3.1.3 silver nitrate solution. 17g/L. A.3.1.4 sodium nitrite solution. 100g/L. A.3.1.5 hydrochloric acid solution. 3 → 10. A.3.1.6 nitric acid solution. 3 → 50. A.3.1.7 barium chloride. 50g/L. A.3.1.8 sodium hydroxide solution. 50g/L. A.3.2 Analysis step A.3.2.1 Take a platinum wire dipped little of this product, a colorless combustion flame, the flame that was yellow. A.3.2.2 3g samples weighed to the nearest 0.1g, was dissolved in 20mL water, remove 1mL, silver nitrate solution was added 2mL, 30s after generating Cyclohexylamino white precipitate of silver nitrate. A.3.2.3 Weigh 0.3g sample, accurate to 0.1g, dissolved in 20mL water, hydrochloric acid and sodium nitrite solution 5mL solution 3mL, Was heated on a water bath for about 15min, removed after cooling, add ether 20mL shaking extraction, the ether layer into the evaporating dish, evaporated on a water bath Removal of the ether, add water 1mL, plus 0.5mL nitric acid on a water bath heated 20min later, evaporated to dryness on a sand bath, no charring. After cooling The residue was dissolved 3mL water was added to a solution of nitric acid and sodium hydroxide solution adjusted pH4.5 ~ 7.0, was added silver nitrate 1mL, a white sink precipitate. Nitric acid was added, a white precipitate was dissolved. A.3.2.4 A.3.2.3 take aqueous layer was extracted after addition of barium chloride solution 1mL, a white precipitate formed. Determination A.4 cyclohexylamino sodium content (dry basis) of A.4.1 Method summary After drying the sample in glacial acetic acid as the solvent, 1-naphthol in the presence of benzene indicator solution, titration with perchloric acid standard solution titration, according to consumption The volume of perchloric acid standard titration solution content was calculated cyclohexylamino sodium. A.4.2 Reagents and materials A.4.2.1 glacial acetic acid. A.4.2.2 perchloric acid standard titration solution. c (HClO4) = 0.1mol/L. A.4.2.3 1- naphthol benzyl indicator solution. 2g/L. 1-naphthol benzene weighed 0.2g, dissolved in glacial acetic acid, diluted to 100mL with glacial acetic acid. A.4.3 Analysis step A.4.3.1 said 0.3g sample taken after drying, accurate to 0.0002g, ice acetic acid 30mL, heated to dissolve, cooled to room temperature, 1-naphthol benzene indicator solution 5 drops to 6 drops of perchloric acid titration standard solution titration solution from yellow to green as the end point. A.4.3.2 measured at the same time, according to the same procedure and the determination of the sample without using the same amount of reagent blank test solution. A.4.4 Calculation Results Cyclohexylamino sodium content (dry basis) of the mass fraction w1, according to equation (A.1) Calculated. w1 = (V1-V2) × c × M m × 1000 × 100% (A.1) Where. V1 --- sample consumed perchloric acid standard titration solution volume in milliliters (mL); V2 --- blank perchloric acid standard titration solution consumption volume in milliliters (mL); Concentration c --- perchloric acid standard titration solution, expressed in moles per liter (mol/L); --- Cyclohexylamino the M sodium molar mass in grams per mole (g/mol), (M = 201.22); M --- the quality of the sample, in grams (g); 1000 --- volume conversion factor. The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Not more than 0.3%. A.5 Sulfate (SO4 meter) measurement A.5.1 Reagents and materials A.5.1.1 hydrochloric acid solution. 3 → 10. A.5.1.2 barium chloride solution. 250g/L. A.5.1.3 sulphate (SO4) standard solution. 0.1mg/mL. A.5.2 Analysis step Weigh 10.0g sample accurate to 0.01g, dissolved in about 60mL of water, placed in 100mL flask (filtered if necessary), diluted with water Release to the mark. Pipette 5mL ± 0.05mL The solution was placed in 50mL colorimetric tube, add 1mL hydrochloric acid solution under shaking Dropping 3mL barium chloride solution, dilute with water to 50mL, shake, place 10min, the turbidity was not greater than the standard turbidity solution. Turbidity standard solution is to take 5mL sulfate standard solution and treated in the same sample at the same time. A.6 pH (100g/L aqueous solution) was determined Conducted in accordance with GB/T 9724's. Measured, weighed 10g sample, accurate to 0.01g, plus carbon dioxide-free water to 100mL Measured after mixing. A.7 Determination of loss on drying A.7.1 Method summary Determination of the amount of discharge at a certain temperature in a sample can be volatile substance. A.7.2 Analysis step It weighs about 10g sample, accurate to 0.0001g, placed in a pre dried to a constant mass of 105 ℃ ± 2 ℃ weighing bottle, paved Layer of 5mm or less. Dried in a thermostatic oven 105 ℃ ± 2 ℃ in 2h ~ 4h, placed in the dryer to cool 30min weighing, until Constant weight. A.7.3 Calculation Results Loss on drying mass fraction w2, according to equation (A.2) Calculated. w2 = m2-m1 m2 × 100% (A.2) Where. M2 --- dried before the mass of the sample, in grams (g); Quality, unit m1 --- after drying the sample in grams (g). The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Not more than 0.05%. A.8 Determination of amino acid A.8.1 Reagents and materials A.8.1.1 TLC plates. silica gel 60 TLC plate, the size of 20cm × 20cm, the coating thickness of about 0.25mm. When using cut Length 12cm × width 5cm, or suitable size. A.8.1.2 eluent. water. ammonia. ethyl acetate. n-propanol = 10.10.20.70 volume ratio mixture. A.8.1.3 amino acid standard solution. each 1mL containing 0.15mg amino acid. Weigh 15mg amino acid, dissolved in water and transferred to 100mL volumetric flask, dilute to the mark. A.8.1.4 sodium hypochlorite solution. 120. A.8.1.5 potassium iodide - starch solution. Weigh 0.75g of potassium iodide, dissolved with 100mL of water, heated to boiling, stirring, adding starch solution (14.3g/L) 35mL, boiled for 2min, cooled use. A.8.2 Instruments and Equipment A.8.2.1 micro injector (flat). 10μL. A.8.2.2 expansion slot. A.8.2.3 spray bottle. A.8.3 Analysis step Weigh 10g sample, accurate to 0.01g, was dissolved in 60mL water, and then placed in 100mL flask, diluted with water to the mark, shake uniform. In the bottom of the TLC plate 1cm impose a pencil line. With micro sample taken 2μL sample solution, point TLC plate painting line. The TLC plate placed in vertical expansion slot, covered, developing solution is not more than drawing a line, when the liquid expands to expand the top TLC plate immediately take Out. Placed in an oven at about 105 ℃ drying 5min, taken out of the hot plate spray solution of sodium hypochlorite, dechlorination is placed in the air circulation, TLC plate to drop below the point of sample KI - When the starch solution was slightly pale blue far too long to avoid dechlorination, then thin Chromatographic plate full spray potassium iodide - starch solution, amino acid spots will appear within 5min observe the spot color should not be deeper than standard. Standard with micro-injector Imbibe 2μL amino acid standard solution, and treated in the same sample at the same time. Determination A.9 cyclohexylamine A.9.1 Reagents and materials A.9.1.1 alkaline disodium edetate solution. Weigh 10g of disodium edetate and sodium hydroxide 3.4g, dissolved in water, and dried Diluted with water to 100mL. A.9.1.2 methyl orange acid solution. Weigh 0.2g of methyl orange and acid 3.5g, add water 100mL, placed on a water bath heated to dissolve, quiet Set more than 24h, filtered before use. A.9.1.3 mixture of chloroform and n-butanol.201. A.9.1.4 mixture of methanol and sulfuric acid. 501. A.9.1.5 cyclohexylamine standard solution. Each ml 0.0025mg cyclohexylamine. Weigh cyclohexylamine 0.1g, accurate to 0.0002g, placed 100mL volumetric flask, add water, 50mL, hydrochloric acid 0.5mL, dissolved diluted with water to the mark. The exact amount taken 5.0mL, another set A 100mL volumetric flask, dilute to the mark, shake. This precise amount of dilution 5.0mL, set 100mL flask, diluted with water Release to the mark. A.9.2 Analysis step Weigh 10g sample, accurate to 0.1g, dissolved in about 60mL of water, placed in 100mL flask, diluted with water to the mark. Imbibe this solution with the standard solution of cyclohexylamine 10mL, 60mL two were placed in a separatory funnel were successively added acetic basic Tetraacetic acid disodium salt solution 3.0mL, 15.OmL mixture of chloroform and n-butanol, shaking 2min, rested, take the chloroform Layer, the chloroform extract of the occupation 10.OmL, 60mL placed in a separatory funnel and the other two, each of the boric acid solution was added methyl orange 2.0mL, Shaking 2min, rested, take the chloroform layers, each adding anhydrous sodium sulfate 1g, shaking, standing, amount of chloroform solution 5.0mL, placed Colorimetric tubes, each a mixture of sulfuric acid and methanol was added 0.5mL, shake. The sample solution can not be significantly deeper than the color standard solution. A.10 dicyclohexylamine test A.10.1 reagents and materials A.10.1.1 chloroform. washed three times, each time water is 1/3 of chloroform, the chloroform layer was separated for measurement. A.10.1.2 sodium hydroxide solution. 40g/L. A.10.1.3 Reagent A. bromophenol blue Weigh 75mg, 60mL water, add sodium bicarbonate solution (8.4g/L) 10mL, and dissolved with stirring to Hydrochloric acid solution (155) adjusted to pH 4.0, diluted with water to 100mL, shake, stored in a cool dark place, use within 48h. A.10.1.4 Reagent B. (1 → 12) 20mL, glacial acetic acid 16.6mL in 100mL flask, diluted with water amount of hydrochloric acid solution to the mark Degree, shake. A.10.2 instruments and equipment A.10.2.1 Spectrophotometer. with 5cm absorption cell. A.10.2.2 separating funnel. 250mL. A.10.3 Analysis steps Weigh 10.0g sample accurate to 0.01g, in 250mL separating funnel, add water to dissolve 100mL, 100mL another amount of water Reagent blank to another separating funnel. Each 10mL sodium hydroxide solution was added, and then were washed sequentially with 10mL, 5mL and 5mL Chloroform extraction were combined chloroform extracts in the other two separating funnel, add water each 100mL, reagent B3.0mL, reagent A1.0mL, shaking 3min, dark for 30min, after standing layer separated chloroform layer is 25mL colorimetric tube, add chloroform To 25mL. At 410nm wavelength, with 5cm absorption cell, chloroform zero, measure the absorbance of the sample solution and reagent blank, Absorbance difference is not greater than 0.20 is qualified. A.11 absorbance value (100g/L solution) Determination A.11.1 instruments and equipment A.11.1.1 ultraviolet-visible spectrophotometer. A.11.1.2 1cm quartz cuvette. A.11.2 Analysis steps Weigh 10g sample, accurate to 0.01g, dissolved in about 60mL of water, placed in 100mL flask, diluted with water to the mark. UV-visible spectrophotometer, cuvette, the absorbance was measured at 270nm wavelength in 1cm quartz. Water zero. A.12 transparency (light transmittance expressed as 100g/L solution) is measured Weigh the sample 10g (accurate to 0.01g), dissolved in about 60mL of water, and then placed in 100mL volumetric flask, dilute to the mark, Shake well. Using a spectrophotometer at 1cm absorption cell transmittance measured at 420nm wavelength. With light transmittance of 100% water. A.13 heavy metals (Pb) Determination A.13.1 Method summary Under weakly acidic conditions, the samples of heavy metals (Pb) with thioacetamide and generated brown-black, lead to the same treatment of (Pb) Comparison of standard solution, to do limited testing. A.13.2 reagents and materials A.13.2.1 thioacetamide solution. Weigh thioacetamide 4g, accurate to 0.1g, dissolved in 100mL of water, placed in refrigerator. Immediately prior to taking this solution 1.0mL added to the mixture in advance by the sodium hydroxide solution (1 25) 15mL, water 5mL and 20mL glycerol composition 5mL, placed on a water bath for 20s, cooling immediately. A.13.2.2 carbon dioxide-free water. A.13.2.3 ammonium acetate buffer, pH = 3.5. Weigh 25.0g of ammonium acetate, 25mL dissolved in water, add 45mL 6mol/L salt Acid, dilute hydrochloric acid or dilute ammonia to adjust pH = 3.5, dilute with water to 100mL. A.13.2.4 Lead (Pb) standard solution. 1μg/mL. This solution was prepared just before use. A.13.3 Analysis steps Weigh 10.0g laboratory samples, accurate to 0.01g, was dissolved in about 60mL carbon dioxide-free water, placed in 100mL volumetric flask Diluted with carbon dioxide-free water to the mark, shake, is the sample solution. Draw the sample solution 12mL, 25mL stoppered placed colorimetric tube, namely A tube is. Draw 10mL 2mL lead standard solution and the sample solution was placed in 25mL colorimetric tube with a stopper, shake, is the B tube (standard). Absorb carbon dioxide-free water and 10mL sample solution 2mL set 25mL colorimetric tube with a stopper, shake, is the C tube (blank). In A, B, C tubes, each added 2mL ammonium acetate buffer solution, shake, respectively dropping 1.2mL acetyl ammonium thiosulfate solution, rapid mixing. With respect to the tube C, B show a light brown pipe. 2min, the color should not be deeper than the pipe A B tube. 5102- 73􀏕 6881 ......

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