GB 29222-2012National food safety standards -- Food additives -- Polyoxyethylene (20) sorbitan monopalmitate (Tween 40) (English PDF)

3.1 Sensory requirements

Shall comply with the provisions of Table 1.

Table 1 sensory requirements

The project requires a test method Color is yellow to orange at room temperature State at room temperature viscous liquid or frozen paste Take the appropriate amount of sample, placed in a clean, dry white porcelain dish, in the natural light to observe the color and status

3.2 Physical and chemical indicators

Shall comply with the provisions of Table 2.

Table 2 Physical and chemical indicators

Item Index Test Method Acid value (in KOH)/(mg/g) <= 2.0 Appendix A A.4 Saponification value (in KOH)/(mg/g) 41 to 52 Appendix A A.5 Hydroxyl value/(in KOH)/(mg/g) 90 to 107 Appendix A A.6 Moisture, w /% <= 3.0 Appendix A A.7 Burning residue, w /% <= 0.25 GB/T 7531a Lead (Pb)/(mg/kg) <= 2 GB 5009.12 Oxyethylene group (calculated as C2H4O), w /% 66.0 to 70.5 GB/T 7385 a The burning temperature is 850 °C ± 25 °C.

Appendix A

Testing method

A.1 Warning

The test procedure specifies that some of the test procedures may lead to dangerous conditions and that the operator 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. The solution used in the test method refers to the aqueous solution when the solvent is not specified.

A.3 Identification test A.3.1 Reagents and materials A.3.1.1 Sodium hydroxide solution. 43 g/L.

A.3.1.2 cobalt thiocyanate solution. 17.4 g of ammonium thiocyanate, 2.8 g of cobalt nitrate, dissolved in water to 100 mL.

A.3.1.3 Hydrochloric acid solution. 23 77.

A.3.2 Identification method A.3.2.1 Take 1 mL of the sample and dissolve in 20 mL of water. Take the solution 10mL, add 5mL cobalt thiocyanate solution, mix, add 5mL three Methyl chloride, shaking and mixing, after standing, the chloroform layer was blue.

A.3.2.2 Take 1 mL of the sample and dissolve in 20 mL of water. Take the solution 5mL, add 5mL sodium hydroxide solution, boil for a few minutes, cooling, Acidified with hydrochloric acid solution, milky white turbidity.

A.3.2.3 take 6mL sample, add 4mL water to mix, at room temperature or below room temperature was jelly.

A.4 Determination of acid value (in KOH) A.4.1 Reagents and materials A.4.1.1 isopropanol.

A.4.1.2 Toluene.

A.4.1.3 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L.

A.4.1.4 phenolphthalein indicator solution. 10g/L.

A.4.2 Analysis steps Weigh about 5g sample, accurate to 0.0002g, placed in a conical flask, adding isopropyl alcohol and toluene 40mL, heated to dissolve. plus Into the 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide titration solution to the solution was pink, keep 30s do not fade for the end.

A.4.3 Calculation of results the acid value w1, expressed as potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g), according to formula (A.1) w1 = V1 × c × M (A.1) where.

V1 --- sodium hydroxide standard titration solution volume of the value 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 greater than 0.2 mg/g.

A.5 Determination of saponification value (in KOH) A.5.1 Reagents and materials A.5.1.1 anhydrous ethanol.

A.5.1.2 Potassium hydroxide solution. 40 g/L.

A.5.1.3 Standard titration solution for hydrochloric acid. c (HCl) = 0.5 mol/L.

A.5.1.4 phenolphthalein indicator solution. 10g/L.

A.5.2 Analysis steps Approximately 2.6 g of the sample was weighed to 0.0002 g, placed in a 250 mL Erlenmeyer flask, 25 mL of 0.02 mL of hydroxide Potassium ethanol solution, connected to the condenser, in the water bath reflux 1h, slightly cold with 10mL anhydrous ethanol leaching condensate tube, remove the conical flask, add Into the 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 pink, Continue titration to red disappears as the end point.

At the same time as the measurement, the same amount of reagent solution was used as a blank test in the same procedure as in the measurement.

A.5.3 Calculation of results the saponification value w2, expressed as potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g), according to formula (A.2) w2 = (V0 - V2) × c × M (A.2) where.

V2 --- sample consumption of hydrochloric acid standard titration solution volume value in milliliters (mL);

V0 --- blank test consumption of hydrochloric acid standard titration solution volume value in milliliters (mL);

c - the exact value of the standard titration solution for hydrochloric acid, 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 greater than 1 mg/g.

A.6 Determination of hydroxyl value (in KOH) A.6.1 Reagents and materials A.6.1.1 pyridine. phenolphthalein as indicator, with c (HCl) = 0.1mol/L hydrochloric acid solution and.

A.6.1.2 n-butanol. Phenolphthalein as an indicator, with potassium hydroxide ethanol standard titration solution (A.6.1.4) and.

A.6.1.3 Acetylating agent. Acetic anhydride and pyridine were mixed in 1 3 and stored in a brown bottle.

A.6.1.4 Potassium hydroxide ethanol standard titration solution. c (KOH) = 0.5mol/L.

A.6.1.5 phenolphthalein indicator solution. 10g/L.

A.6.2 Analysis steps Weigh about 2g sample, accurate to 0.0002g, placed in 250mL grinding conical flask, add 5mL ± 0.02mL acetylation agent, Connect the condenser to reflux on a water bath for 1 h. Add 10 mL of water from the top of the condenser to the conical flask and continue to heat for 10 min but 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 phenolphthalein finger Liquid, with potassium hydroxide ethanol standard titration solution titration to the solution was pink that is the end.

At the same time as the measurement, the same amount of reagent solution was used as a blank test in the same procedure as in the measurement.

To correct the free acid, weigh about 10g of the sample, accurate to 0.01g. Placed in a conical flask, add 30mL of pyridine, add 5 drops of phenolphthalein Indicator solution, titrated with potassium hydroxide ethanol titration solution to the solution was pink.

A.6.3 Calculation of results Hydroxyl value w3, calculated as potassium hydroxide (KOH), the value in milligrams per gram (mg/g), according to formula (A.3) w3 = (V0 - V3) × c × M V4 × c × M m1 (A.3) where.

V3 --- sample consumption of potassium hydroxide ethanol standard titration solution volume value in milliliters (mL);

V0 --- blank test consumption of potassium hydroxide ethanol standard titration solution volume value, the unit is ml (mL);

V4 --- corrected free acid consumption of potassium hydroxide ethanol standard titration solution volume value in milliliters (mL);

c - potassium hydroxide ethanol standard titration solution concentration of the exact value in moles per liter (mol/L);

m - value of the mass of the sample when measured by the hydroxyl value, in grams (g);

m1 --- corrected free acid determination of the sample quality of the value of the unit 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 4 mg/g.

A.7 Determination of Moisture Weigh about 0.6g of sample, accurate to 0.0002g. Placed in a 25mL beaker, add a small amount of chloroform, dissolved in heat and transferred to 25mL volumetric flask, rinse the beaker several times with chloroform, into the volumetric flask, diluted to the scale. Measure 5 mL ± 0.02 mL Sample solution, according to GB/T 6283 direct charge 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%.