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GB 1886.232-2016 English PDF

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GB 1886.232-2016: National Food Safety Standard -- Food Additives -- Sodium Carboxymethyl Cellulose
Status: Valid
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GB 1886.232-2016179 Add to Cart 3 days National Food Safety Standard -- Food Additives -- Sodium Carboxymethyl Cellulose Valid

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Basic data

Standard ID: GB 1886.232-2016 (GB1886.232-2016)
Description (Translated English): National Food Safety Standard -- Food Additives -- Sodium Carboxymethyl Cellulose
Sector / Industry: National Standard
Classification of Chinese Standard: X42
Word Count Estimation: 9,939
Date of Issue: 2016-08-31
Date of Implementation: 2017-01-01
Older Standard (superseded by this standard): GB 1904-2005
Regulation (derived from): State Health and Family Planning Commission Notice No.11 of 2016
Issuing agency(ies): National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 1886.232-2016: National Food Safety Standard -- Food Additives -- Sodium Carboxymethyl Cellulose


---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 additive - Sodium carboxymethyl cellulose National Standards of People's Republic of China National Food Safety Standard Food additives Sodium carboxymethyl cellulose 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 1904-2005 "food additive sodium carboxymethyl cellulose." This standard compared with GB 1904-2005, the main changes are as follows. --- Increased content of sodium and the indicator ethanol sodium; --- Modify the drying loss, viscosity, chloride (as NaCl) and the indicator of lead; --- Remove the index requirements of iron, heavy metals. National Food Safety Standard Food additives Sodium carboxymethyl cellulose

1 Scope

This standard applies to cellulose, sodium hydroxide and monochloroacetic acid or its sodium salt as the main raw material, the food additive sodium carboxymethyl cellulose. 2 molecular formula, relative molecular mass and structural formula Formula 2.1 [C6H7O2 (OH) x (OCH2COONa) y] n n. degree of polymerization x. 1.5 ~ 2.8 y. the degree of substitution of 0.2 to 1.5 xy = 3.0 2.2 formula R = H or CH2COONa 2.3 relative molecular mass n is about 100, > 17,000 (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 White or slightly yellow color Status fibrous or granular powder The sample is placed in the appropriate uniform white porcelain plate, under the 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 Carboxymethylcellulose sodium content, w /% ≥ 99.5 Appendix A A.3 Viscosity (mass fraction of 2% aqueous solution) a/(mPa · s) ≥ 5.0 Appendix A A.4 The degree of substitution of 0.20 to 1.50 in Appendix A A.5 pH (10g/L aqueous solution) 6.0-8.5 A, Appendix A.6 Loss on drying, w /% ≤ 8.0 GB 5009.3 direct drying b Sodium ethanol, w /% ≤ 0.4 Appendix A A.7 Chloride (as NaCl), w /% ≤ 0.5 Appendix A A.8 Sodium, w /% ≤ 12.4 A.9 in Appendix A Arsenic (As)/(mg/kg) ≤ 2.0 GB 5009.76 Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.75 When a viscosity (mass fraction of 2% aqueous solution) ≥2000mPa · s should use the mass fraction of 1% aqueous solution measured. b drying temperature of 105 ℃ ± 2 ℃, drying time is 2h.

Appendix A

Testing method A.1 General Provisions Unless otherwise specified in this standard, the purity of the reagents used should be analytically pure, the standard titration solution, impurity measurement standard solution, preparations and Products, should be GB/T 601, GB/T 602, preparation, test water should be consistent with GB/T 6682 provisions prescribed in the three water GB/T 603's. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution. A.2 Identification Test A.2.1 Reagents and materials A.2.1.1 hydrochloric acid. A.2.1.2 potassium iodide - iodine solution. Take 0.5g of iodine and potassium iodide 1.5g dissolved in 25mL water. A.2.1.3 copper sulfate (CuSO4 · 5H2O) solution. 20g/L. A.2.2 Preparation of test solution Take 2g sample was placed in 100mL of warm water, stir, and continue stirring until jelly, cooled to room temperature. A.2.3 Identification method A.2.3.1 about taking the test solution 30mL, add 2 drops to 3 drops of potassium iodide - iodine solution, does not appear blue. A.2.3.2 about taking the test solution 50mL, 10mL copper sulfate solution was added, resulting in a fluffy pale blue precipitate. A.2.3.3 with hydrochloric moist platinum wire, the first burning flame on colorless to colorless, then dipped a little test solution, colorless flame burning in fire That flame was bright yellow. A.3 Determination of sodium carboxymethyl cellulose content Sodium carboxymethyl cellulose sodium content equal to 100% minus the mass fraction of alcohol (w1) and chloride content (w2). A.4 Determination of viscosity A.4.1 Instruments and Equipment A.4.1.1 viscometer. Value or Analog. A.4.1.2 glass. diameter of about 90mm, a height of about 122mm, in diameter from top to bottom, capacity of about 500mL. A.4.1.3 water bath. A.4.1.4 mechanical stirrer. stainless steel or glass, connected to the load at a different energy to 900r/min ± 100r/min of the rotation becomes Speed motor on. A.4.2 Analysis step Weigh 5.0g (formulated mass fraction of 1% of the test solution) or 10.0g (formulated mass fraction of 2% of the test solution) sample accurate To 1mg. Join them in the glass 495.0g (formulated mass fraction of 1% of the test solution) or 490.0g (formulated mass fraction of 2% Test solution) of water, put the blender to the glass, stirred the leaves around 10mm from the bottom of the cup, stirring was initiated and slowly added to the sample, adjusting the stirring Speed to 900r/min ± 100r/min, stirring 2h, as the sample is not completely dissolved, then continue stirring 0.5h, remove stirrer, glass Cups were placed in a water bath at 25 ℃ ± 0.2 ℃ 1h, if not permanent solution to 25 ℃ ± 0.2 ℃, the need to continue after the thermostat to 25 ℃ ± 0.2 ℃, Removed manually stirred 10s, with a viscosity measured viscosity. First viscometer rotor immersed in the sample solution, and then start the viscometer rotation about 1min, Stable value to be displayed after the reading. A.4.3 Calculation Results A.4.3.1 value viscometer Direct reading, is the viscosity value of the sample. A.4.3.2 pointer viscometer Viscosity η, the value in mPas (mPa · s) said, according to the formula (A.1) Calculated. η = S × k (A.1) Where. S --- rotational viscometer pointer readings in milli-Pascal seconds (mPa · s); And the rotational speed of the rotor coefficient chosen k --- when measured. The test results should indicate the concentration of the test solution and the number of rotor and rotor speed. The test results of the arithmetic mean of the parallel determination results shall prevail, the two independent determination results under repeatability conditions measured absolute difference Value must not exceed 5% to 10% of the arithmetic mean. A.5 Determination of the degree of substitution A.5.1 Method summary The sample was washed with ethanol to remove soluble salts, dried and burned at high temperature, and the residue of sodium oxide, sodium hydroxide dissolved in water to generate, plus excess Sulfuric acid standard titration solution, titration with sodium hydroxide standard solution titrate the excess sulfuric acid, obtained by calculating each anhydrous glucose unit carboxylase The average value of methyl groups, that is, the degree of substitution. A.5.2 Reagents and materials A.5.2.1 ethanol. A.5.2.2 ethanol. amount of ethanol 90mL, diluted with water to 100mL. A.5.2.3 sulfuric acid standard titration solution. c 12H2SO4 ÷ = 0.1mol/L. A.5.2.4 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L. A.5.2.5 methyl red indicator solution. 1g/L. A.5.3 Instruments and Equipment A.5.3.1 sintered glass crucible. filter plate aperture 15μm ~ 40μm. A.5.3.2 porcelain crucible. 20mL ~ 25mL. A.5.4 Analysis step Weigh about 1.5g sample was placed in a glass sand crucible, washed with pre-heated to 50 ℃ ~ 70 ℃ in ethanol several times (each time to fill Glass sand crucible) until add 1 drop of potassium chromate solution and the filtrate 1 drop of silver nitrate solution was brick red for the completion of washing, on the contrary should continue to wash Polyester, generally washed 5 times. Finally a wash with absolute ethanol, the sample is moved after washing the sand core crucible, at 120 ℃ ± 2 ℃ drying 2h (At around 1h, the sand core sample crucible gently knock loose). Stamped within a desiccator, cool to room temperature. Weigh about 1g sample to the nearest 0.0002g, placed in a porcelain crucible in the furnace charring not to smoke, add 300 ℃ high temperature furnace, heated to 700 ℃ ± 25 ℃, insulation 15min, turn off the power, cooling to below 200 ℃, moved within a 250mL beaker, add 100mL of water and 50mL ± 0.05mL sulfuric acid standard Quasi-titration solution, the beaker was placed on a heating furnace, slowly boiling 10min, add 2 drops to 3 drops of methyl red indicator solution, cooled, neutralized with sodium hydroxide Standard Solution titration to red just faded. A.5.5 Calculation Results The degree of substitution xD.S, according to equation (A.2) and formula (A.3) Calculated. cB = V1 × c1-V2 × c2 (A.2) xD.S = 0.162cB 1-0.080cB (A.3) Where. Millimoles carboxymethyl --- cB of the sample, in units of millimoles per gram (mmol/g); V1 --- volume of sulfuric acid standard titration solution, in milliliters (mL); C1 --- the actual concentration of sulfuric acid standard titration solution, expressed in moles per liter (mol/L); Volume V2 --- sodium hydroxide standard titration solution, in milliliters (mL); The actual concentration c2 --- sodium hydroxide standard titration solution, expressed in moles per liter (mol/L); M --- the quality of the sample, in grams (g); Cellulose --- 0.162 mmol of a glucose unit mass in grams per millimole of (g/mmol); Quality --- 0.080 mmol sodium carboxymethyl group in units of grams per mmol (g/mmol). The results represent two decimal. The arithmetic average of the results of two parallel determination of the measurement result, two parallel measurement results If the absolute difference is not more than 0.02. A.6 pH measurement of Potentiometric measuring method or measuring pH 10g/L sample solution with a pH test paper. According to GB/T 9724 regulations measured by potentiometric method Be given, weigh about 1.0g sample accurate to 0.01g, add 100mL of carbon dioxide-free water, after mixing was measured. Determination A.7 ethanol sodium A.7.1 Reagents and materials A.7.1.1 sulfuric acid. A.7.1.2 glycolic acid. A.7.1.3 acetone. A.7.1.4 sodium chloride. A.7.1.5 glacial acetic acid. A.7.1.6 2,7- dihydroxynaphthalene solution. Weigh 0.1g of 2,7-dihydroxynaphthalene was dissolved in 1000mL concentrated sulfuric acid, the solution was allowed to stand until the yellow color disappeared. The solution was stored in a brown reagent bottle, valid for one month. A.7.1.7 aluminum foil. A.7.2 Instruments and Equipment A.7.2.1 Spectrophotometer. A.7.2.2 electronic balance, accuracy 0.0001g. A.7.2.3 water bath. A.7.2.4 flask. 25mL, 100mL. A.7.3 Analysis step A.7.3.1 sample processing 0.5g sample is accurately weighed, was added 100mL beaker with 5mL of glacial acetic acid completely infiltrated, then 5mL of water was added, with a glass rod Stir until completely dissolved (typically 15min required), the stirring process is slowly added 50mL of acetone, and then added 1g of sodium chloride, stirred Mixed minutes, sodium carboxymethylcellulose ensure complete precipitation. Quantitative filter paper, filter paper wetted with a small amount of acetone, and the filtrate was collected 100mL volumetric flask. Also with 30mL acetone and accelerate the transfer of solid cake is washed, then with acetone to volume, shake. A.7.3.2 preparation of standard solution of glycolic acid Accurately weighed at room temperature drier 24h glycolic acid 0.100g (accurate to 1mg), placed in 100mL volumetric flask Dissolved in water and dilute to volume, the solution was valid for one month. Respectively of the solution 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL were added 5 100mL flasks, each flask Add water to a total volume of 5mL, plus 5mL glacial acetic acid, acetone with constant volume, referred to as No.1 to No.5. Take 2.0mL sample solution and standard solution 1 to No. 5 were added 25mL volumetric flask, the flask placed in a boiling unsealed 20min acetone bath was removed, and then removed from the boiling water bath and cooled. Each flask was added 5mL2,7- dihydroxynaphthalene, are mixed Then absorbed 15mL2,7- dihydroxynaphthalene was added, mixed evenly. With aluminum foil to seal each bottle capacity. Each flask placed in a boiling water bath In 20min, cooled and then removed with sulfuric acid to volume, shake. A.7.4 standard curve With a spectrophotometer to No. 1 solution as the control, using 1cm cuvette, the absorbance was measured in the standard series solution at 540nm And the absorbance of the sample solution, standard curve. A.7.5 Calculation Results Sodium ethanol mass fraction w1, according to equation (A.4) Calculated. w1 = 12.9 × m1 (100-b) × m0 (A.4) Where. --- 12.9 (molar mass of sodium molar mass of ethanol/glycolic acid) × 10; Mass m1 --- found in the standard curve of glycolic acid, in milligrams (mg); b --- Loss on drying mass fraction,%; m0 --- sample mass, in grams (g). A.8 Determination of chloride A.8.1 Method summary Samples were dissolved in water, titration with standard silver nitrate titration, indicate the end of a potentiometer. Was added a solution of hydrogen peroxide to degrade Viscosity. A.8.2 Reagents and materials A.8.2.1 nitrate. A.8.2.2 hydrogen peroxide. A.8.2.3 standard silver nitrate titration solution. c (AgNO3) = 0.1mol/L. A.8.3 Instruments and Equipment A.8.3.1 potentiometric titrator. with a silver electrode and a saturated calomel electrode (double salt bridge). A.8.3.2 microburette. 10mL. A.8.4 Analysis step Said drying 2h learn the 105 ℃ ± 2 ℃ 2g sample, accurate to 0.0002g, placed in 250mL beaker, add water and 100mL 5mL of hydrogen peroxide. The beaker was placed in a steam bath for heating with occasional stirring to obtain a non-viscous solution. If the viscosity of the solution after 20min Has not been completely degraded, plus 5mL of hydrogen peroxide and heated until completely degraded. Cooling beaker, add 100mL of water and 10mL of nitric acid, is set On the titrator magnetic stirrer, a solution of silver nitrate with microburette standard titration solution to the potential end. A.8.5 Calculation Results Chloride content (as NaCl) mass fraction w2 meter, according to equation (A.5) Calculated. w2 = c × V × M m × 100% (A.5) Where. C --- standard silver nitrate solution concentration, in units of moles per liter (mol/L); Volume V --- silver nitrate titration standard solution, in milliliters (mL); --- The M NaCl mmoles mass in grams per millimole of (g/mmol) (M = 0.05845); M --- the quality of the sample, in grams (g). Calculation result to one decimal place. The arithmetic average of the results of two parallel determination of the measurement result, two parallel measurement results If the absolute difference is not more than 0.06%. A.9 Determination of sodium Sodium mass fraction w3, according to equation (A.6) Calculated. w3 = 0.023 × xD.S 0.162 0.080xD.S × 100% (A.6) Where. xD.S --- samples degree of substitution; Sodium --- 0.023 mmol mass in grams per millimole of (g/mmol); Cellulose --- 0.162 mmol of a glucose unit mass in grams per millimole of (g/mmol); Quality --- 0.080 mmol sodium carboxymethyl group in units of grams per mmol (g/mmol).
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