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GB 13481-2011 English PDF

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GB 13481-2011: The national food safety standards of food additives sorbitan monostearate ester (Span 60)
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GB 13481: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
GB 13481-2011English229 Add to Cart 3 days [Need to translate] The national food safety standards of food additives sorbitan monostearate ester (Span 60) Valid GB 13481-2011
GB 13481-2010English399 Add to Cart 3 days [Need to translate] National food safety standards of food additives -- Sorbitan monostearate (Span 60) Obsolete GB 13481-2010
GB 13481-1992English319 Add to Cart 3 days [Need to translate] Food additive Sorbitan monostearate (Span 60) Obsolete GB 13481-1992

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Basic data

Standard ID GB 13481-2011 (GB13481-2011)
Description (Translated English) The national food safety standards of food additives sorbitan monostearate ester (Span 60)
Sector / Industry National Standard
Classification of Chinese Standard X42
Classification of International Standard 67.220.20
Word Count Estimation 10,164
Date of Issue 2011-11-21
Date of Implementation 2011-12-21
Older Standard (superseded by this standard) GB 13481-2010
Regulation (derived from) The Ministry of Health in 2011 Notice No. 26
Issuing agency(ies) Ministry of Health of the People's Republic of China
Summary This Chinese standard applies to sorbitan stearic acid as raw materials, by esterification reaction of a food additive sorbitan monostearate (Span 60).

GB 13481-2011: The national food safety standards of food additives sorbitan monostearate ester (Span 60)


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The national food safety standards of food additives sorbitan monostearate ester (Span 60) National Food Safety Standard Food additives sorbitan monostearate (Span 60) Issued on. 2011-11-21 2011-12-21 implementation National Standards of People's Republic of China People's Republic of China Ministry of Health issued

Foreword

This standard replaces GB 13481-2010 "national food safety standards for food additives sorbitan monostearate (Span 60). " This standard compared with GB 13481-2010, the main changes are as follows. - Changes A.8.2 Analysis step. This standard replaces the standards previously issued as follows. --GB 13481-1992; --GB 13481-2010. National Food Safety Standard Food additives sorbitan monostearate (Span 60)

1 Scope

This standard applies to stearic acid and sorbitan as raw material, obtained by esterification of food additives sorbitan monostearate Ester (Span 60).

2 Technical Requirements

2.1 Sensory requirements. comply with Table 1. Table 1 Sensory requirements Project requires test methods Pale yellow color take appropriate laboratory sample, placed in a clean, dry white porcelain dish, In natural light, visually observed. Powdery or solid mass organization status 2.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Fatty acids, w /% 71 ~ 75 in Appendix A A.4 Polyols, w /% 29.5 ~ 33.5 Appendix A A.5 Acid value (in dollars KOH)/(mg/g) ≤ 10 Appendix A A.6 Saponification value (in dollars KOH)/(mg/g) 147 ~ 157 Appendix A A.7 A hydroxyl value (KOH meter)/(mg/g) 235 ~ 260 Appendix A A.8 Water, w /% ≤ 1.5 A.9 in Appendix A Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.10 Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.11

Appendix A

Testing method A.1 Warning Some test procedures prescribed test method can lead to dangerous situations. The operator shall take appropriate safety and health practices. A.2 General Provisions Unless otherwise indicated in the analysis using only confirm three analytical grade reagents and water GB/T 6682-2008 stipulated. Test Methods standard titration solution, when measured impurity standard solution, preparations and products, with no other requirements noted, According to GB/T 601, the provisions of GB/T 602 and GB/T 603 of the preparation. A.3 Identification Test A.3.1 Determination of fatty acid value A.3.1.1 Reagents and materials A.3.1.1.1 ethanol. A.3.1.1.2 sodium hydroxide standard titration solution. c (NaOH) = 0.5mol/L. A.3.1.1.3 phenolphthalein indicator solution. 10g/L. A.3.1.2 analysis step Weigh about 3g A.4.3.2 Coagulum in the D, accurate to 0.001 g of, placed in a conical flask, 50mL of anhydrous ethanol solution, will Heating when necessary. Add 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide standard titration solution until the solution was pink, holding 30s do not fade As the end point. A.3.1.3 Calculation Results Fatty acid value w1, potassium hydroxide (KOH) and its value in milligrams per gram (mg/g) expressed by the formula (A.1) Calculated. VcM = (A.1) Where. Numerical V-- sodium hydroxide standard titration solution (A.3.1.1.2) volume in milliliters (mL); Accurate c-- sodium hydroxide standard titration solution concentration value in units of moles per liter (mol/L); m-- sample mass value in grams (g); M-- numerical molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference is not more than 0.5 (Mg/g). A.3.1.4 result of the judgment The acid number of the fatty acid is recovered 190 (mg/g) ~ 220 (mg/g). A.3.2 Determination of fatty acid crystallization point According to GB/T 7533 carried out. Take about 3g A.4.3.2 of coagulum D as a sample. The recovered fatty acid crystallization point should be ≥ 53 ℃. A.3.3 polyols color test Take about 2g A.5.2 of goo E, added 2mL catechol solution (100g/L) (using now), mix, plus 5mL sulfur Sour mix, should be significantly red or reddish-brown. A.4 Determination of Fatty Acids A.4.1 Method summary Samples by saponification hydrolysis, after acidification resulting fatty acids and polyols, isolated and concentrated and dried by repeated extraction to give back Quality received fatty acids, fatty acid weighed to calculate the mass fraction. A.4.2 Reagents and materials A.4.2.1 potassium hydroxide. A.4.2.2 ethanol (95%). A.4.2.3 petroleum ether. A.4.2.4 sulfuric acid solution. 12. A.4.3 Analysis step A.4.3.1 saponification. Weigh about 25g laboratory samples, accurate to 0.01g. Placed in 500mL flask, 250mL of ethanol (95%) And 7.5g of potassium hydroxide. Connected to the condenser, water bath heated at reflux for 2h. The saponification was transferred to 800mL beaker, with about 200mL The flask was washed with water and transferred to the beaker. The beaker was placed in a water bath until the evaporation of volatile ethanol Yat do. Regulating body with hot water solution Volume to about 250mL, the solution A. A.4.3.2 acidification, extraction separation. adding sulfuric acid solution to the solution A under heating with stirring to precipitate coagulum, and then added an excess of about 10% sulfuric acid solution, cooling the layers separated. The upper layer was transferred to a pre-coagulated at 80 ℃ constant quality 250mL beaker, hot 20mL Washed with water three times, and after cooling the lower wash solution were combined in 500mL separatory funnel, extracted with 100mL of petroleum ether 3 times, allowed to stand for minutes Floor. The lower layer solution was transferred to a 800mL beaker B; petroleum ether extracts were combined in a second separatory funnel 500mL, 3 times with 100mL Water. The lower aqueous wash solution B merged with solution C, reserved for determination of the content of the polyol used; Transfer the upper petroleum ether extracts in Sheng Ning The solid material in the beaker, placed in a water bath and concentrated to 100mL, and dried at 80 deg.] C to a constant mass to afford recovered coagulum D as fatty acid the quality of. After weighing coagulum D for the determination of fatty acid value. A.4.4 Calculation Results Fatty mass fraction w2, expressed in%, according to equation (A.2) Calculated. twenty one mm = ×% (A.2) Where. m1--250mL beaker quality value in units of grams (g); m2--250mL beaker added value was solidified D mass in grams (g); m-- sample mass value in grams (g). The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference is not more than 1%. Determination A.5 polyol A.5.1 Reagents and materials A.5.1.1 ethanol. A.5.1.2 potassium hydroxide solution. 100g/L. A.5.2 Analysis step With potassium hydroxide solution and the solution obtained A.4.3.2 C to pH 7 (using pH paper test). The solution was placed in a water bath Evaporated to a white crystalline precipitate. Then 4 times with 150mL hot ethanol extraction residue of the polyol, and the combined extracts were washed with G4 glass filter funnel, washed with absolute ethanol. The filtrate was transferred to another 800mL beaker, placed in a water bath concentrated to about 100mL. Transferred again to advance at 80 ℃ constant quality 250mL beaker, and evaporation was continued until sticky. At 80 ℃ dried to constant mass to give E as the viscous material quality recycled polyols. After weighing goo E polyol used color test. A.5.3 Calculation Results Polyol mass fraction w3, expressed in%, according to equation (A.3) Calculated. twenty one mm = ×% (A.3) Where. m1--250mL beaker mass in grams (g); Quality m2--250mL beaker plus goo E, expressed in grams (g); m - A.4.4 The sample mass value in grams (g). The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference is not more than 1%. A.6 Determination of acid value A.6.1 Reagents and materials A.6.1.1 isopropanol. A.6.1.2 toluene. A.6.1.3 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L. A.6.1.4 phenolphthalein indicator solution. 10g/L. A.6.2 Analysis step Weigh about 2.5g laboratory samples, accurate to 0.000 1g, set conical flask, isopropyl alcohol and toluene each 40mL, heated to Dissolved. Add 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide standard titration solution until the solution was pink, holding 30s does not fade as the end point. A.6.3 Calculation Results An acid value of w4, potassium hydroxide (KOH) and its value in milligrams per gram (mg/g) expressed by the formula (A.4) Calculated. V cM = (A.4) Where. V1 - Numerical sodium hydroxide standard titration solution (A.6.1.3) volume in milliliters (mL); c - accurate sodium hydroxide standard titration solution concentration value in units of moles per liter (mol/L); m1 - mass of the sample value in units of grams (g); M-- numerical molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference is not more than 0.2 (Mg/g). A.7 Determination of saponification value A.7.1 Reagents and materials A.7.1.1 ethanol. A.7.1.2 ethanolic potassium hydroxide. 40g/L. A.7.1.3 hydrochloric acid standard titration solution. c (HCl) = 0.5mol/L. A.7.1.4 phenolphthalein indicator solution. 10g/L. A.7.2 Analysis step Weigh about 2g laboratory samples, accurate to 0.000 1g, placed in 250mL grinding mouth Erlenmeyer flask, (25 ± 0.02) mL hydroxide Ethanol solution of potassium, connection condenser, water bath heated at reflux for 1 h, coolish rinsed with 10mL ethanol condenser, remove Erlenmeyer flask, add 5 drops of phenolphthalein indicator solution, titration with hydrochloric acid standard titration solution to the solution of the red just disappeared, the test solution was heated to boiling. If there is pink, continue titration to the disappearance of the red is the end. 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.7.3 Calculation Results Saponification value w5, potassium hydroxide (KOH) and its value in milligrams per gram (mg/g) expressed by the formula (A.5) Calculated. () VV cM = (A.5) Where. V 2-- sample consumption hydrochloric acid standard titration solution (A.7.1.3) the value of the volume, in milliliters (mL); Numerical volume V0-- blank test consumption hydrochloric acid standard titration solution (A.7.1.3), in milliliters (mL); Accurate c-- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L); m2 - Numerical sample mass, in grams (g); M-- numerical molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference is not more than 1 (mg/g). A.8 Determination of hydroxyl value A.8.1 Reagents and materials A.8.1.1 pyridine. phenolphthalein as an indicator, with hydrochloric acid solution (1110) and. A.8.1.2 butanol. phenolphthalein as an indicator, the standard titration with potassium hydroxide in ethanol solution. A.8.1.3 acetylating agent. acetic anhydride in pyridine by mixing 13, stored in a brown bottle. A.8.1.4 ethanol potassium hydroxide standard titration solution. c (KOH) = 0.5mol/L. A.8.1.5 phenolphthalein indicator solution. 10g/L. A.8.2 Analysis step Weigh about 1.2g laboratory samples, accurate to 0.0001g, placed in 250mL grinding mouth Erlenmeyer flask, (5 ± 0.02) mL acetylating agent, Connecting a condenser, water bath heated at reflux for 1h. Condenser was added 10mL of water from the upper end of the conical flask and heating continued for 10min after, Cooled to room temperature. 15mL washing condenser with n-butanol, remove the condenser, and then rinse the bottle wall 10mL of n-butanol. Was added 8 drops of phenolphthalein means Shows, washed with ethanol and potassium hydroxide standard titration solution titrated to a solution pink is the end. 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. To correct the free acid, weigh about 10g laboratory samples, accurate to 0.01g. Placed in a conical flask, 30mL of pyridine was added 5 Drops of phenolphthalein indicator solution, titration with a standard solution of potassium hydroxide in ethanol solution was titrated to a pink. A.8.3 Calculation Results Hydroxyl value w6, potassium hydroxide (KOH) and its value in milligrams per gram (mg/g) expressed by the formula (A.6) Calculated. () VV cM V cM mm = (A.6) Where. V3 - sample consumption of potassium hydroxide in ethanol standard titration solution (A.8.1.4) the value of the volume, in milliliters (mL); V0-- blank test of ethanol consumption of potassium hydroxide standard titration solution (A.8.1.4) the value of the volume, in milliliters (mL); V4-- correction free acid consumption of potassium hydroxide in ethanol standard titration solution (A.8.1.4) the value of the volume, in milliliters (mL); Accurate c-- potassium hydroxide in ethanol Standard Solution value in units of moles per liter (mol/L); Sample value quality of hydroxyl values measured in grams (g) - m3; m0-- corrected sample mass of the free acid value when measured in units of grams (g); M-- numerical molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference of not more than 4 (mg/g). A.9 Determination of Moisture Weigh about 0.6g laboratory samples, accurate to 0.0002g. Placed in 25mL beaker was added a small amount of chloroform and dissolved by heating switch Move 25mL volumetric flask, rinse the beaker several times with chloroform, be transferred to a volumetric flask, dilute to the mark. Weighed (5 ± 0.02) mL The sample solution, according to GB/T 6283 direct charge method. The arithmetic average of the results of two parallel determination for reporting results. Two parallel determination results of absolute difference is not more than 0.05%. A.10 Determination of Arsenic According to GB/T 5009.76 Gutzeit method. Press the "wet digestion" process sample amount of (10 ± 0.02) in the sample solution mL (measured phase When the laboratory sample to 1.0g). Limits formulated solution. pipette pipette (3 ± 0.02) mL arsenic (As) standard solution (equivalent to 3μg As), and treated in the same sample at the same time. A.11 Determination of Lead A.11.1 colorimetry (Arbitration Act) According to GB/T 5009.75 conduct. Processing of samples. Weigh about 2.5g laboratory samples, accurate to 0.000 1g, a 50mL crucible, First at a low temperature carbonization, and then at 500 ℃ ~ 550 ℃ ashing, after cooling, was added 5mL nitric acid solution (11), followed by stirring to dissolve, plus 10mL water was transferred to a 25mL volumetric flask, dilute to the mark, shake. A.11.2 Atomic Absorption Spectrometry Carried out according to GB 5009.12. According to GB/T 5009.75 "the dry digestion" process samples. When using graphite furnace atomic absorption spectrometry, visual The sample having a sample solution diluted.

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