Food additive - Sorbitan tristearate (Sipan 65) detection

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A. 7. Determination of saponification value (calculated by KOH)

A.7.1 Reagents and materials

A.7.1.1  Anhydrous ethanol

A.7.1.2; Potassium hydroxide ethanol solution: 40g/L

A.7.1.3 Hydrochloric acid standard titration solution: c (HC1)=0.5mol/L

A.7.1.4 Phenolphthalein indicator solution: 10g/L

A.7.2 Analysis Steps

Weigh approximately 2g of the sample, accurate to 0.0002g, and place it in a 250mL ground conical flask. Add 25mL ± 0.02mL of potassium hydroxide ethanol solution, connect the condenser tube, reflux in a boiling water bath for 1 hour, cool slightly, rinse the condenser tube with 10mL of anhydrous ethanol, remove the conical flask, add 5 drops of phenolphthalein indicator solution, and titrate with hydrochloric acid standard titration solution until the red color of the solution has just disappeared. Heat the test solution until it boils. If pink appears, continue titration until the red disappears, which is the endpoint

At the same time as the measurement, perform a blank test using the same amount of reagent solution without adding a sample, following the same steps as the measurement

A.7.3 Result Calculation

The saponification value w5 is calculated in potassium hydroxide (KOH), and the value is expressed in milligrams per gram (mg/g). Calculate according to equation (A.5):

In the equation:

V0- The volume of hydrochloric acid standard titration solution consumed by the sample, in milliliters (mL)

V3- Value of the volume of hydrochloric acid standard titration solution consumed in the blank test, in milliliters (mL)

C - The accurate value of the concentration of hydrochloric acid standard titration solution, in moles per liter (mol/L)

M - numerical value of the sample mass, in grams (g)

M - The numerical value of the molar mass of potassium hydroxide, in grams per mole (g/mo) [M=56.109]

Take the arithmetic mean of the results of two parallel measurements as the reported result. The absolute difference between the results of two parallel measurements should not exceed 1mg/g

A.8 Determination of hydroxyl value (calculated by KOH)

A.8.1 Reagents and materials

A.8.1.1 Pyridine: Using phenolphthalein as an indicator, neutralize with hydrochloric acid solution (1+110).

A.8.1.2; N-butanol: Using phenolphthalein as an indicator, neutralize with potassium hydroxide ethanol standard titration solution

A.8.1.3 Acetylation agent: Mix acetic anhydride and pyridine in a ratio of 1+3 and store 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

Weigh approximately 1.2g of the sample to the nearest 0.0002g, place it in a 250mL ground conical flask, add 5mL ± 0.02mL of acetylation agent, connect the condenser tube, and heat and reflux on a water bath for 1 hour.

. Add 10mL of water from the upper end of the condenser tube to a conical flask, continue heating for 10 minutes, and then cool to room temperature. Wash the condenser tube with 15mL of n-butanol, remove the condenser tube, and then rinse the bottle wall with 10mL of n-butanol. Add 8 drops of phenolphthalein indicator solution and titrate with potassium hydroxide ethanol standard titration solution until the solution turns pink, which is the endpoint

At the same time as the measurement, perform a blank test using the same amount of reagent solution without adding a sample, following the same steps as the measurement

To correct for free acids, weigh approximately 10g of the sample to the nearest 0.01g. Place in a conical flask, add 30mL pyridine, add 5 drops of phenolphthalein indicator solution, and titrate with potassium hydroxide ethanol standard titration solution until the solution turns pink

A.8.3 Result Calculation

The hydroxyl value w6 is calculated in potassium hydroxide (KOH), and the value is expressed in milligrams per gram (mg/g). Calculate according to equation (A.6):

In the equation:

V4- The volume of potassium hydroxide ethanol standard titration solution consumed by the sample, in milliliters (mL)

V0- Value of the volume of potassium hydroxide ethanol standard titration solution consumed in the blank test, in milliliters (mL)

V5- The numerical value for correcting the volume of potassium hydroxide ethanol standard titration solution consumed by free acid, in milliliters (mL)

C - The accurate value of the concentration of potassium hydroxide ethanol standard titration solution, in moles per liter (mol/L)

m - The numerical value of the sample mass during the determination of hydroxyl value, in grams (g)

m5- The numerical value of the sample mass during the calibration of free acid measurement, in grams (g)

M - The numerical value of the molar mass of potassium hydroxide, in grams per mole (g/mol) [M=56.109]

Take the arithmetic mean of the results of two parallel measurements as the reported result. The absolute difference between the results of two parallel measurements should not exceed 4mg/g

A.9 Determination of Moisture

Weigh approximately 0.6g of the sample to the nearest 0.0002g. Place in a 25mL beaker, add a small amount of trichloromethane, heat and dissolve, and transfer to a 25mL volumetric flask. Rinse the beaker several times with trichloromethane, then transfer to a volumetric flask and dilute to the mark. Measure 5mL ± 0.02mL of the sample solution and measure it according to the direct coulometric method in GB/T6283

Take the arithmetic mean of the results of two parallel measurements as the reported result. The absolute difference between the results of two parallel measurements should not exceed 0.05%

A.10 Determination of freezing point

A.10.1 Instruments and equipment

Glass tube: length 100mm, diameter 25mm, wall thickness 1mm.

A.10.2 Analysis Steps

Add about 5g of sample to the glass tube, slowly heat until the sample dissolves, and let the temperature be slightly higher than the freezing point of 15 ℃~20 ℃. Place the glass tube in a transparent glass bottle (150mm long, 70mm diameter), cover the glass bottle with a perforated lid, place the standard thermometer in the melted sample, and stir. If cooling is required, slowly stir until the mercury column of the thermometer rises for 30 seconds without change. Stop stirring and place the thermometer in the middle of the sample. Observe the rise of the mercury column and read the maximum temperature value of the mercury column as the freezing point

 

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