GB 25552-2010 English PDF

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GB 25552-2010: National food safety standards of food additives sorbitan monopalmitate (Span 40)
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Basic data

Standard ID: GB 25552-2010 (GB25552-2010)
Description (Translated English): National food safety standards of food additives sorbitan monopalmitate (Span 40)
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Classification of International Standard: 67.220.20
Word Count Estimation: 10,150
Date of Issue: 2010-12-21
Date of Implementation: 2011-02-21
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 applies to palmitic acid and sorbitan esterification reaction of a food additive sorbitan palmitate (Span 40).

GB 25552-2010: National food safety standards of food additives sorbitan monopalmitate (Span 40)

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National food safety standards of food additives sorbitan monopalmitate (Span 40) National Standards of People's Republic of China National standards for food safety Food Additives Sorbitan Monopalmitate (Span 40) 2010-12-21 release 2011-02-21 Implementation Issued by the Ministry of Health of the People's Republic of China

Foreword

Appendix A of this standard is a normative appendix. National standards for food safety Food Additives Sorbitan Monopalmitate (Span 40)

1 Scope

This standard applies to the palmitic acid and sorbitan esterification reaction of the food additive sorbitan monopalmitate (Span 40).

2 normative reference documents

The documents cited in this standard are indispensable for the application of this standard. Any reference to the date of the document, only the date of the edition This applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard.

3 technical requirements

3.1 sensory requirements. should be consistent with the provisions of Table 1. Table 1 sensory requirements The project requires a test method Color pale yellow Tissue state waxes Take appropriate laboratory samples, placed in clean, dry white Porcelain plate, in the natural light, visual observation 3.2 Physical and chemical indicators. should be consistent with the provisions of Table 2. Table 2 Physical and chemical indicators Item Index Test Method Fatty acids, w /% 63 ~ 71 Appendix A, A.4 Polyols, w /% 33 to 38 Appendix A, A.5 Acid value (in KOH)/(mg/g) ≤ 7 Appendix A A.6 Saponification value (in KOH)/(mg/g) 140 to 155 Appendix A A.7 Hydroxyl value (in KOH)/(mg/g) 270 to 305 Appendix A, A.8 Moisture, w /% ≤ 1.5 Appendix A, A.9 Burning residue, w /% ≤ 0.50 Appendix A. A.10 Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.11 Lead (Pb)/(mg/kg) ≤ 2 Appendix A. A.12

Appendix A

(Normative appendix) Testing method A.1 Warning Some of the test procedures specified in the test method may result in a hazardous situation. Operators should take appropriate safety and protective measures. A.2 General provisions Unless otherwise stated, only the reagents identified as analytical reagents and the tertiary water specified in GB/T 6682-2008 are used in the analysis. Standard titration solution used in the test method, standard solution for the determination of impurities, preparations and articles, in the absence of other requirements, GB/T 601, GB/T 602 and GB/T 603. A.3 Identification test A.3.1 Determination of fatty acid value A.3.1.1 Reagents and materials A.3.1.1.1 anhydrous 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 steps Weigh about 3gA.4.3.2 in the coagulation D, accurate to 0.001g, placed in a conical flask, add 50mL of anhydrous ethanol dissolved, must To be heated. Add 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide titration solution to the solution was pink, keep 30s does not fade for end. A.3.1.3 Calculation of results The fatty acid value w1 is expressed in milligrams per gram (mg/g) in terms of potassium hydroxide (KOH) and is calculated according to the formula (A.1) w1 = VcMm (A.1) Where. V - sodium hydroxide standard titration solution (A.3.1.1.2) in milliliters (mL); c - the exact value of sodium hydroxide standard titration solution concentration in moles per liter (mol/L); m - the mass of the sample, in grams (g); M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.5 mg/g. A.3.1.4 Judgment of results The recovered fatty acid value should be 210 mg/g to 225 mg/g (in KOH). A.3.2 Polyol color test Take about 2gA.5.2 in the sticky material E, add 2mL catechol solution (100g/L) (now with the current), mix, plus 5mL sulfur Acid mixed, should be red or reddish brown. A.4 Determination of Fatty Acids A.4.1 Methodological Summary The samples were hydrolyzed by saponification, and the fatty acids and polyols formed after acidification were separated by repeated extraction and concentrated to obtain a recovered fat The quality of the acid is calculated and the mass fraction of the fatty acids is calculated. 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. 1 2. A.4.3 Analysis steps A.4.3.1 Saponification. Weigh about 25g of laboratory samples, accurate to 0.01g. Placed in a 500 mL flask and 250 mL of ethanol was added (95%) and 7.5 g of potassium hydroxide. Connect the condenser and place it in a water bath for 2h. The saponification product was transferred to a 800 mL beaker The flask was washed with about.200 mL of water and transferred to the beaker. Place the beaker in a water bath and evaporate until the ethanol evaporates. Adjust with hot water The volume of the solution is about 250 mL, as solution A. A.4.3.2 Acidification, Extraction Separation. Add sulfuric acid solution to Solution A with heating and stirring to precipitate the coagulum and add an excess of about 10% The sulfuric acid solution is cooled and layered. The supernatant was transferred to a 250 mL beaker which had a constant mass at 80 ° C and three times with 20 mL Hot water washing, cooling the lotion and the lower solution after the merger in a 500mL separatory funnel, 3 times with 100mL petroleum ether extraction, Floor. The lower layer B was transferred to a 800 mL beaker; the combined petroleum ether extract was added to a second 500 mL separatory funnel, 100 mL of water. The lower layer of water washing solution and solution B into solution C, retained for the determination of polyol content; transfer of the upper layer of petroleum ether extract In a beaker, placed in a water bath and concentrated in 100 mL, dried at 80 ° C until the mass was constant, and the recovered coagulum D was obtained as The quality of fatty acids. The coagulated substance D after weighing is used for the determination of the fatty acid value. A.4.4 Calculation of results The mass fraction of fatty acids w2, expressed in%, is calculated according to equation (A.2). w2 = m2-m1m x 100% (A.2) Where. m1 --- 250mL beaker mass value in grams (g); m2 --- 250mL beaker plus solid D value of the value, in grams (g); m - the mass of the sample, in grams (g). The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 1%. A.5 Determination of polyol A.5.1 Reagents and materials A.5.1.1 anhydrous ethanol. A.5.1.2 Potassium hydroxide solution. 100 g/L. A.5.2 Analysis steps The solution C to pH 7 obtained in A.4.3.2 was neutralized with potassium hydroxide solution (tested with pH paper). Place the solution in a water bath Evaporated to white crystals. The polyol in the residue was then extracted twice with 150 mL of hot ethanol and the combined extracts were washed with G4 Glass funnel filter, anhydrous ethanol wash. The filtrate was transferred to another 800 mL beaker and concentrated in a water bath to about 100 mL. again Transferred to a 250 mL beaker in a constant mass at 80 ° C and continue to evaporate to a viscous shape. Dry at 80 ° C until the mass is constant and get sticky The quality of the complex E as the recovered polyol. After weighing the viscous material E for the polyol color test. A.5.3 Calculation of results Polyol mass fraction w3, expressed in%, calculated according to formula (A.3). w3 = m2-m1m x 100% (A.3) Where. m1 --- 250mL beaker quality, in grams (g); m2 --- 250mL beaker plus viscous material quality, in grams (g); m --- A.4.4 The mass of the sample in grams, in grams (g). The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations 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 steps Weigh about 2.5g of laboratory samples, accurate to 0.0001g, placed in a conical flask, adding isopropyl alcohol and toluene 40mL, heated to make it Dissolve. Add 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide titration solution to the solution was pink, keep 30s does not fade for the end. A.6.3 Calculation of results The acid value w4, expressed as potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g), calculated according to formula (A.4) w4 = V1cMm1 (A.4) Where. V1 --- sodium hydroxide standard titration solution (A.6.1.3) volume of the value in milliliters (mL); c - the exact value of sodium hydroxide standard titration solution concentration in moles per liter (mol/L); m1 --- the mass of the sample, in grams (g); M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not greater than 0.2 mg/g. A.7 Determination of saponification value A.7.1 Reagents and materials A.7.1.1 anhydrous ethanol. A.7.1.2 Potassium hydroxide ethanol solution. 40 g/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 steps Weigh about 2g of laboratory samples, accurate to 0.0001g, placed in 250mL mill vial, add (25 ± 0.02) mL of hydroxide Potassium ethanol solution, connected to the condenser, placed in a water bath heated reflux 1h, slightly cold with 10mL anhydrous ethanol leaching condenser, remove the cone Bottle, add 5 drops of phenolphthalein indicator solution, titrated with hydrochloric acid standard titration solution to the red just disappeared, heating the test solution to boiling. If there is powder Red, continue to titration to the red disappearance is the end point. At the same time as the measurement, the same amount of the reagent solution was used as a blank test in the same manner as in the measurement. A.7.3 Calculation of results The saponification value w5, expressed as potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g), calculated according to formula (A.5) w5 = (V0-V2) cM m2 (A.5) Where. V2 --- sample consumption of hydrochloric acid standard titration solution (A.7.1.3) volume of the value in milliliters (mL); V0 --- blank test consumption of hydrochloric acid standard titration solution (A.7.1.3) volume of the value in milliliters (mL); c - the exact value of the standard titration solution for hydrochloric acid, in moles per liter (mol/L); m2 --- the mass of the sample, in grams (g); M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not greater than 1 mg/g. Determination of hydroxyl value of A.8 A.8.1 Reagents and materials A.8.1.1 Pyridine. neutralized with hydrochloric acid solution (1 110) using phenolphthalein as an indicator. A.8.1.2 n-butanol. phenol phenol as the indicator, with potassium hydroxide ethanol standard titration solution and. A.8.1.3 Acetylating agent. Acetic anhydride and pyridine were mixed in 1 3 and stored in a brown bottle. A.8.1.4 Potassium hydroxide ethanol standard titration solution. c (KOH) = 0.5mol/L. A.8.1.5 phenolphthalein indicator solution. 10g/L. A.8.2 Analysis steps Approximately 1 g of laboratory sample was weighed to 0.0001 g, placed in a 250 mL Erlenmeyer flask, (5 ± 0.02) mL of acetylated Agent, connected to the condenser, placed in a water bath heated reflux 1h. Add 10 mL of water from the top of the condenser to the conical flask and continue heating for 10 min After cooling to room temperature. Rinse the condenser with 15 mL of n-butanol, remove the condenser, and rinse the wall with 10 mL of n-butanol. Add 8 drops of phenol Phthalate indicator solution, titration with potassium hydroxide ethanol titration solution to the solution was pink is the end point. At the same time as the measurement, the same amount of the reagent solution was used as a blank test in the same manner as in the measurement. To calibrate the free acid, weigh about 10g of laboratory samples, accurate to 0.01g. Placed in a conical flask, add 30 mL of pyridine, add 5 drops of phenolphthalein indicator solution, titration with potassium hydroxide ethanol titration solution to the solution was pink. A.8.3 Result calculation The hydroxyl value w6 is expressed in milligrams per gram (mg/g) in terms of potassium hydroxide (KOH) and is calculated according to formula (A.6) w6 = (V0-V3) cM m3 V4cM m0 (A.6) Where. V3 --- sample consumption of potassium hydroxide ethanol standard titration solution (A.8.1.4) volume of the value in milliliters (mL); V0 --- blank test consumption of potassium hydroxide ethanol standard titration solution (A.8.1.4) volume of the value in milliliters (mL); V4 --- corrected free acid consumption of potassium hydroxide ethanol standard titration solution (A.8.1.4) volume of the value in milliliters (mL); c - potassium hydroxide ethanol standard titration solution concentration of the exact value in moles per liter (mol/L); m3 --- value of the value of the test value of the value of gold, the unit is grams (g); m0 --- corrected free acid determination of the quality of the sample value, the unit is grams (g); M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109]. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 4 mg/g. A.9 Determination of moisture Weigh about 0.6g of laboratory samples, accurate to 0.0002g. Placed in 25mL beaker, add a small amount of trichloromethane heated and dissolved Transfer to a 25 mL volumetric flask, rinse the beaker several times with chloroform, and transfer it to the volumetric flask and dilute it to the mark. Measure (5 ± 0.02) mL The sample solution, according to GB/T 6283 in the direct electricity method. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.05%. A.10 Determination of burning residue According to GB/T 7531. The firing temperature is (850 ± 25) ° C. A.11 Determination of arsenic According to GB/T 5009.76 arsenic spot method. The samples were processed by the "wet digestion" method and the solution was taken (10 ± 0.02) mL (Equivalent to 1.0g of laboratory samples). (3 ± 0.02) mL of arsenic (As) standard solution (equivalent to 3 μgAs) with a pipette. Sample processing. A.12 Determination of lead (Pb) A.12.1 Colorimetric method (arbitration law) According to GB/T 5009.75. Sample treatment. Weigh about 2.5g of laboratory samples, accurate to 0.0001g, placed in 50mL crucible In the crucible, carbonized at a low temperature and then ashed at 500 ° C to 550 ° C. After cooling, 5 mL of nitric acid solution (1 1) was added and stirred to dissolve Solution, add 10mL of water transferred to the 25mL volumetric flask, diluted with water to the mark, shake. A.12.2 Atomic Absorption Spectrometry According to GB 5009.12. According to GB/T 5009.75 "dry digestion" treatment samples. When using graphite furnace atomic absorption spectrometry, Depending on the sample, the sample solution is properly diluted. ......

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