Food Additives - Detection of Attapulgite Clay

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Some reagents used in the inspection methods of this standard are toxic or corrosive, and caution must be exercised during operation! If splashed onto the skin, rinse immediately with water, and in severe cases, seek immediate treatment

A.2 General Provisions

Unless otherwise specified, only reagents confirmed as analytical pure and Grade III water specified in GB/T6682-2008 shall be used in the analysis.

. The standard titration solution, impurity determination standard solution, formulation, and product used in the test method shall be prepared in accordance with the provisions of GB/T601, GB/T602, and GB/T603 unless otherwise specified; When no solvent is specified, the solution used refers to an aqueous solution

A.3 Identification Test

A.3.1 X-ray Diffraction Spectroscopy Identification

The X-ray diffraction spectrogram of the attapulgite clay should be basically consistent with Figure B.1 in Appendix B

A.3.2; Magnesium oxide (MgO) content test

The mass fraction of magnesium oxide measured by X-ray fluorescence spectrometer should not be less than 6%

A.4 Determination of decolorization rate

A.4.1 Method Summary

Take a certain amount of neutralized soybean oil, add a certain amount of sample for decolorization, and measure the absorbance of the decolorized oil.

. Calculate the decolorization rate as a percentage based on the decrease in absorbance

A.4.2 Reagents and Materials

A.4.2.1 Soybean Oil: Clarified and fresh neutralized soybean oil with an absorbance range of 0.2 to 0.4

A.4.2.2 Quick qualitative filter paper

A.4.3 Instruments and Equipment

A.4.3.1 Spectrophotometer: equipped with a 1cm colorimetric dish.

A.4.3.2 Constant temperature magnetic stirrer

A.4.4 Analysis Steps

Weigh 0.4000g of the sample that has been dried at 105 ℃± 3 ℃ and place it in a 50mL dry grinding conical flask. Add 40.00g of soybean oil, insert a thermometer into the oil and seal it with a sleeve. Place it on a preheated constant temperature magnetic stirrer, stir while heating, and control the heating time to about 10min. The stirring intensity should be based on the swirling motion of the entire oil sample. Keep the thermometer submerged in the oil sample at all times, and start timing when the temperature rises to 110 ℃. Maintain the temperature at 115 ℃± 5 ℃ and stir for 25 minutes for decolorization. After decolorization, filter with double-layer medium speed qualitative filter paper while hot into a 50mL dry beaker. Place the clarified oil sample filtered above on a spectrophotometer and measure the absorbance of the oil sample at a wavelength of 520nm (using a 1cm colorimetric dish with water as a reference, correcting for zero position). Simultaneously measure the absorbance of undiluted soybean neutralizing oil at a wavelength of 520nm

A.4.5 Result Calculation

The decolorization rate X1 is calculated according to equation (A.1):

In the equation:

A0- The absorbance of the non decolorized oil sample at a wavelength of 520nm

A1- The absorbance of the decolorized oil sample at a wavelength of 520nm

The experimental results shall be based on the arithmetic mean of the parallel measurement results, and the absolute difference between the two parallel measurement results shall not exceed 2%

A.5 Determination of Moisture

The determination of moisture shall be determined using the direct drying method according to GB5009.3, and the drying temperature shall be 105 ℃± 3 ℃

A.6; Determination of free acid (calculated as H2SO4)

A.6.1 Method Summary

Extract the free acid from the sample with water, use phenolphthalein as an indicator, titrate with sodium hydroxide standard titration solution, and calculate the free acid content of the sample

A.6.2 Reagents and Materials

A.6.2.1 Sodium hydroxide standard titration solution: c (NaOH)=0.02mol/L

A.6.2.2 Phenolphthalein indicator solution: Weigh 0.1g of phenolphthalein (C20H14O4) and dissolve it in 100mL of anhydrous ethanol

A.6.2.3 Medium speed qualitative filter paper

A.6.3 Analysis Steps

Weigh approximately 1g of the sample, accurate to 0.0001g, place it in a 150mL beaker, add 50mL of water, heat and boil for 3 minutes.

. Filter in a 250mL conical flask, wash the beaker and filter paper with hot water 4-5 times (with a total water consumption of about 50mL), cover with a rubber stopper with a caustic asbestos drying tube, and cool to room temperature. Remove the rubber stopper, rinse the conical bottle wall with water, add 2-3 drops of phenolphthalein indicator solution, and immediately titrate with sodium hydroxide standard titration solution until it turns slightly red and remains unchanged for 30 seconds as the endpoint. Simultaneously conduct a blank experiment

A.6.4 Result calculation

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