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GB 30612-2014: [Including 2020XG1] National Food Safety Standard -- Food Additives -- Polydimethyl Siloxane (PDMS) and Its Emulsion
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GB 30612-2014: [Including 2020XG1] National Food Safety Standard -- Food Additives -- Polydimethyl Siloxane (PDMS) and Its Emulsion

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(Food additive and polydimethylsiloxane emulsion) National Standards of People's Republic of China National standards for food safety Food additives polydimethylsiloxane and its emulsions Released.2014-04-29 2014-11-01 implementation People's Republic of China National Health and Family Planning Commission released National standards for food safety Food additives polydimethylsiloxane and its emulsions

1 Scope

This standard applies to food additives polydimethylsiloxane and its emulsion. Note. Polydimethylsiloxane is a fully methylated linear siloxane polymer prepared by hydrolysis of a mixture of dimethyldichlorosilane and a small amount of trimethylchlorosilane. Polydimethylsiloxane emulsion is a food additive polydimethylsiloxane as raw material, plus deionized water, accessories (see Appendix A), the emulsification processing. 2 polydimethylsiloxane structural formula, molecular formula, relative molecular mass 2.1 Structural formula Where n is from 90 to 410. 2.2 Molecular formula C3H9Si (C2H6OSi) nSiOC3H9. 2.3 Relative molecular mass 6832.356 ~ 30548.196 (according to.2011 international relative atomic mass).

3 technical requirements

3.1 sensory requirements Sensory requirements shall comply with the requirements of Table 1. Table 1 sensory requirements project index Polydimethylsiloxane polydimethylsiloxane emulsion Testing method Colorless colorless transparent milky white Traces of viscous liquid viscous liquid Take appropriate sample in a clean, dry and transparent container Under natural light, observe its color and traits 3.2 Physical and chemical indicators Physical and chemical indicators should be consistent with the provisions of Table 2. Table 2 Physical and chemical indicators project index Polydimethylsiloxane polydimethylsiloxane emulsion Testing method The solubility was tested by means of Test B.3.1 in Appendix B Stability - Test B.6 Refractive index (25 ℃) 1.400 ~ 1.405 - B.3.2 Relative density (25 ℃/25 ℃) 0.964 ~ 0.977 - GB/T 5009.2 Drying reduction (mass fraction) /% ≤ 0.5 - B.4 Viscosity (25 ℃)/cSt 100 ~ 1500 - B.5 Nonvolatile matter (mass fraction) /% ≥ - 10 B.7 Lead (Pb)/(mg/kg) ≤ 1 5 GB 5009.12a Total arsenic (calculated as As)/(mg/kg) ≤ - 2 GB/T 5009.11a a sample treatment is dry ashing.

Appendix A

Accessories The emulsifiers, stabilizers, thickeners and preservatives used in polydimethylsiloxane emulsions are as follows. Mono-, diglycerin fatty acid esters (oleic acid, linoleic acid, linolenic acid, palmitic acid, behenic acid, stearic acid, lauric acid), polyoxyethylene sorbitan mono Stearate (also known as Tween 60), sorbitan monolaurate (also known as the Secretary 20), sorbitan monostearate (also known as the Secretary 60), the sea Propylene glycol aluminate, propylene glycol, silica, polyoxyethylene sorbitan tristearate, polyoxyethylene stearate, sucrose fatty acid ester, yellow Raw rubber (also known as Hansen gum), methyl cellulose, sodium polyacrylate, polyethylene glycol, sodium carboxymethyl cellulose, benzoic acid and its sodium salt, sorbic acid and its Potassium salt.

Appendix B

Testing method B.1 Warning Some of the reagents in this standard test method are toxic and corrosive and the operator should be careful to spill on the skin. Wash should be treated immediately. B.2 General provisions The reagents and water used in this standard, when not specified in other requirements, refer to the analytical reagent and the secondary water specified in GB/T 6682. B.3 Identification test Note. Polydimethylsiloxane commercial formulations usually contain silicone gel, pure polymer can be.20000r/min centrifugal separation of the preparation of silicone gel obtained. The silica gel contained in the polydimethylsiloxane should be removed by centrifugation before testing the properties (refractive index, relative density, viscosity) of the polydimethylsiloxane. B.3.1 Solubility Take 10 mL of the test solvent (water/ethanol or aliphatic solvent/aromatic hydrocarbon solvent) in 25 mL of colorimetric tubes, add 1 mL (Polydimethylsiloxane or polydimethylsiloxane emulsion), shaken for 30 s, and the results were observed after 3 min. Polydimethylsiloxy The alkane should be insoluble in ethanol and water, soluble in most of the aliphatic solvents (such as petroleum ether, n-hexane, etc.) and aromatic hydrocarbon solvents (such as benzene, toluene, etc.). Polydimethylsiloxane emulsions can be dissolved in water and ethanol. B.3.2 Determination of refractive index B.3.2.1 Instruments and equipment Abbe's Refractometer. B.3.2.2 Reagents and materials B.3.2.2.1 Ethanol. B.3.2.2.2 Ethyl ether. B.3.2.3 Analysis steps Before the measurement, the refractometer should be calibrated with two pure water, and the refractive index of the secondary pure water is shown in Table B.1. Adjusted by the Abbe's Refractometer Water, so that the temperature is 25 ℃ ± 0.5 ℃. Open the two prism of the refractometer, with absorbent cotton dipped in ethanol or ether wipe. Drop 1 drop ~ 2 drops of sample (if necessary) to quickly close the prism on the lower prism, no air bubbles. Adjust the reflector to the light source at 25 ° C Fixed 15min, by the eyepiece observation, turn the spiral to the visual field is divided into two parts of light and shade, light compensation compensator knob, so that the two boundaries clear, its points The boundary is just above the intersection of the objective lens. Check and record the temperature and scale on the scale, read the value of the refractive index. Measure and repeat Reading 2 times, the average of three readings is the refractive index of the sample. Table B.1 Refractive index of secondary pure water temperature Refractive index 10 1.3335 15 1.3332 20 1.3329 25 1.3325 30 1.3320 40 1.3305 B.4 Determination of dry reduction The flat type weighing bottle (Φ65mm × 30mm) was placed in an oven, dried at 150 ℃ to constant weight, and the sample was inhaled with latex dropper, Add 4 g to 5 g (accurate to 0.0002 g) in a constant weight weighing flask. And placed in an oven at 100 ° C ± 2 ° C for 3 h and then gradually Raise the oven temperature to 150 ° C for 4 h, remove and place it in a desiccator and cool to room temperature and weigh. The mass fraction w1 (%) for drying reduction is calculated according to formula (B.1) w1 = m3-m1 m2-m1 × 100% (B.1) Where. m3 --- flat type weighing bottle constant weight after the mass value and the quality of the sample after drying, the unit is grams (g); m1 --- flat type weighing bottle constant weight after the value of the unit, in grams (g); m2 --- flat type weighing bottle constant weight after the value of the quality and the value of the sample value, in grams (g). B.5 Determination of viscosity B.5.1 Instruments and equipment Wu's viscometer, the choice of capillary diameter of 2.00mm 0.04mm No. 3 viscometer. Viscometer must be fixed on the bracket to protect The viscometer is vertical and the position of each tube is shown in Figure B.1. The unit is in millimeters Description. A --- sphere A; B --- sphere B; C --- sphere C; 1 --- tube 1; 2 --- tube 2; 3 --- tube 3; T1 --- scale line T1; T2 --- scale line T2. Figure B.1 Ubbelohde viscometer B.5.2 Reagents and materials Viscosity standard oil. B.5.3 Analysis steps B.5.3.1 Calibration of viscometer Determine the viscosity of the standard oil with a known viscosity v (as far as possible the choice of viscosity and standard samples of the test sample, secondary or primary reference material) The viscosity coefficient of the instrument. (See Figure B.1) to make it perpendicular to the vertical line 30 °, the ball B placed under the capillary, from the tube 1 guide Into the test sample to make it exceed the lowest scale line, while ensuring that the sample in the viscometer vertical placement will not exceed the highest scale line, to ensure that U There is no air at the bottom of the tube. Place the viscometer in the bath for a sufficient period of time to bring the test sample to an equilibrium temperature, Tube 3, take the sample from tube 2 to the middle of sphere C. Remove the ball from tube 2 and move the finger from tube 3 to tube 2 until the sample drops to the capillary The bottom end. Remove the finger from the tube 2 and record the time that the liquid level drops from the tick line T1 to the tick line T2 to exactly 0.1s. The whole time Should be controlled at 80s ~ 100s. The viscosity coefficient k is calculated according to equation (B.2). k = t1 (B.2) Where. v - the viscosity of the standard oil, in units of cSt (cSt); t1 --- standard oil consumption time, in seconds (s). B.5.3.2 Determination of viscosity of polydimethylsiloxane Place the test sample in the viscometer and then use the same method as the calibration phase to derive the test sample consumption time t2. Viscosity in terms of vs, the value of centis (cSt) said, according to formula (B.3). vs = k × t2 (B.3) Where. k --- viscosity coefficient, in units of centis per second (cSt/s); t2 --- is the test sample consumption time, in seconds (s). B.6 Determination of stability Take two graduated centrifugal tubes, add 5mL polydimethylsiloxane emulsion sample, symmetrically into the centrifuge, to 3000r/min ± 50r/min After centrifugation for 30min, visually observe the sample in the centrifuge tube, the emulsion should be no demulsification phenomenon, the liquid should be No oil and water separation. B.7 Determination of nonvolatile content The flat type weighing bottle (Φ65 × 30mm) was placed in an oven, dried at 120 ℃ to constant weight, and the sample was inhaled with a latex dropper. 4g ~ 5g (accurate to 0.0002g) in constant weight weighing bottle. And placed in an oven at 100 ° C ± 2 ° C for 3 hours and then at 30 min Gradually raise the oven temperature to 120 ℃ for 2h, remove and place in the dryer to cool to room temperature and then weighed. The nonvolatile content is calculated as mass fraction w2 by equation (B.4) w2 = m3-m1 m2-m1 × 100% (B.4) Where. m3 --- flat type weighing bottle constant weight after the mass value and the amount of sample after drying the mass value, the unit is grams (g); m1 --- flat type weighing bottle constant weight after the mass value, the unit is grams (g); m2 --- flat type weighing bottle constant weight after the mass value and the amount of sample mass, in grams (g). ...