Some standard content:
National Standard of the People's Republic of China
Food additive
Sunset yellow aluminum lake
1 Subject content and scope of application
GB 6227.2--1995
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of food additive sunset yellow aluminum lake. This standard applies to the pigment lake generated by the reaction of food additive sunset yellow and aluminum hydroxide. This product can be added to food as a colorant.
Molecular formula C1H,2N,O,S2
Relative molecular weight 408.41 (according to the 1991 international relative atomic mass) 2 Reference standards
Preparation of standard solution for titration analysis (volume analysis) GB/T 601
Chemical reagents
GB/T602
Chemical reagents
Preparation of standard solution for impurity determination
Chemical reagents
Preparation of preparations and products used in test methods GB/T 603
GB/T 6682
GB/T 8450
GB 6227. 1
3 Technical requirements
Specifications and test methods for water used in analytical laboratoriesDetermination of arsenic in food additives
Sunset yellow
Food additives
3.1 Appearance: orange-yellow powder.
3.2 The quality indicators of food additive sunset yellow aluminum lake shall meet the requirements of the following table: %
Main content (as color acid)
Heating loss (135℃±2℃)
Insoluble matter in hydrochloric acid and ammonia water
Water-soluble chloride and sulfate (as sodium salt) Secondary dye
Arsenic (As)
Heavy metal (as Pb)
Approved by the State Bureau of Technical Supervision on August 17, 1995 128
Implementation on July 1, 1996
4 Test method
GB 6227.2--1995
The reagents and water used in this standard refer to analytical pure reagents and grade 3 water specified in GB/T6682 unless otherwise specified. The standard solutions, impurity standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 respectively when no other requirements are specified.
4.1 Appearance
Measure by visual inspection.
4.2 Identification
4.2.7 Reagents and materials
a. Hydrochloric acid (GB/T622);
b. Potassium dihydrogen phosphate (GB/T1274): 13.6g/L solution: Preparation: Weigh 13.6g of potassium dihydrogen phosphate and dissolve it in water, dilute to about 900mL, then use 70mL of about 40g/L sodium hydroxide solution to adjust the solution to pH7, place it in a 1000mL volumetric flask, and dilute to the scale. Ammonia (GB/T631): (1+2) solution;
Hydrochloric acid (GB/T622): (1+3) solution;
Sodium hydroxide (GB/T629): 40g/L and 100g/L solution Sunset yellow aluminum lake standard sample: content ≥10.0%. f.
4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Analysis steps
4.2.3.1 Weigh about 0.5g of sample, dissolve in 5mL of concentrated hydrochloric acid, place in a 500mL volumetric flask, add potassium dihydrogen phosphate solution to the scale, shake well, then accurately draw 2mL and place in a 50mL volumetric flask, and then dilute to the scale with potassium dihydrogen phosphate solution. The maximum absorption wavelength of the solution should be 482±2nm.
4.2.3.2 Weigh about 0.1g of the sample, add 5mL of hydrochloric acid solution, and heat in a water bath for about 5min, shake to dissolve, the solution is clear, orange-yellow solution, cool, neutralize with ammonia solution, the solution gradually turns into a yellow colloidal precipitate. 4.2.3.3 Weigh about 0.1g of the sample, add 5mL of 100g/L sodium hydroxide solution, heat in a water bath for 5min and shake to dissolve, the solution is clear, orange-yellow solution, cool, neutralize with hydrochloric acid solution to neutral, and form a yellow colloidal precipitate. 4.3 Determination of sunset yellow aluminum lake content
4.3.1 Titanium trichloride titration method
4.3.1.1 In alkaline medium, the azo group in the dye is reduced and decomposed into amino compounds by titanium trichloride, and the percentage of the dye is calculated according to the consumption of titanium trifluoride standard titration solution. 4.3.1.2 Reagents and materials
Ammonium ferrous sulfate (GB/T661)
Hydrochloric acid (GB/T622),
Titanium trichloride;
Trisodium citrate (GB/T3-1298);
Ammonium thiocyanate (GB/T660): 200g/L solution; Sulfuric acid (GB/T625): (1+9), (1+1) solution; Potassium dichromate (GB/T642): c(1/6K,Cr0,)=0.1mal/L standard solution: Titanium trichloride standard solution: c(1/3TiCl)=0.1mo1/L, the preparation method is shown in Appendix A of GB6227.1; h.
Carbon dioxide in cylinders.
4.3.1.3 Analysis steps
Weigh about 7g of sample, accurate to 0.0002g + add (1+9) sulfuric acid solution 80mL, stir and dissolve at 40-50℃, transfer to 129
GB 6227.2-1995
250mL volumetric flask, dilute to scale with freshly boiled water that has been cooled to room temperature, shake well and accurately pipette 50mL, place in a 500mL conical flask, add 30B of trisodium citrate and 200mL of water, assemble the instrument according to Figure 1 in GB6227.1, heat to boiling while passing carbon dioxide gas flow under the liquid surface, and titrate with titanium trichloride standard titration solution until colorless as the end point. 4.3.1.4 Expression of analysis results
The mass percentage content of sunset yellow aluminum lake (X1) is calculated according to formula (1): X = y·c×0,1021 ×100 +
Where: V
The volume of titanium trichloride standard solution consumed by the titration sample, mL; The actual concentration of titanium trichloride standard solution, mol/L; (1
The mass of sunset yellow aluminum lake (in terms of color acid) equivalent to 1.00mL titanium trichloride standard solution [e (1/3TiCla) == 1.000mol/L] in grams:
mThe mass of the sample, g.
4.3.1. 5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1%, and the arithmetic mean shall be taken as the determination result. 4.3.2 Spectrophotometric colorimetric method
4.3.2.1 Method summary
After the sample and the standard sample with known content are dissolved in water, their absorbance is measured at the maximum absorption wavelength, and then the content of the sample is calculated.
4.3.2.2 Reagents and materials
a. Sodium hydrogen tartrate (HG/T 3—1300); b. Sunset yellow aluminum lake standard sample: content ≥10.0%. 4.3.2.3 Instruments and equipment
Spectrophotometer;
Colorimetric III: 10mm.
4.3.2.4 Analysis steps
a Preparation of sunset yellow aluminum lake standard solution
Weigh 0.500g of sunset yellow aluminum lake standard product, accurate to 0.0002g, add 20mL of water and 2g of sodium hydrogen tartrate, heat to 90℃, transfer to a 500mL volumetric flask after dissolution, dilute to scale, shake well, accurately pipette 10mL, and transfer to a 250mL volumetric flask. , dilute to the mark, shake and hook.
b. Preparation of sunset yellow aluminum lake test solution Weighing and operation methods are the same as those for the preparation of standard sample solution. c. Operation
Measure the absorbance of the standard sample solution and the test solution at a wavelength of 482±2nm using 10mm colorimetric solution on a spectrophotometer.
Use water as the reference solution.
4.3.2.5 Expression of analysis results
The mass percentage content of sunset yellow aluminum lake (X,) is calculated according to formula (2): X
Where: A--absorbance of test solution; A,--absorbance of standard sample solution;
GB 6227.2--1995
X, mass percentage of sunset yellow aluminum lake standard sample (titanium trichloride method). 4.3.2.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 2%, and the arithmetic mean shall be taken as the determination result. The above determination method uses the titanium trichloride titration method as the arbitration method. For daily inspection, any one of them can be selected according to the conditions. 4.4 Determination of heating loss
Same as 4.4 in GB6227.1.
4.5 Determination of insoluble matter content in hydrochloric acid and ammonia 4.5.1 Reagents and materials
Hydrochloric acid (GB/T622);
Hydrochloric acid (GB/T622): (3+7) solution;
Ammonia (GB/T631): (4+96) solution
Silver nitrate (GB/T670): c(AgNO,)=17g/L. d.
4.5.2 Analysis steps
Weigh about 2g of sample, accurate to 0.01g, and place it in a 600mL beaker. Add 20mL of water and 20mL of concentrated hydrochloric acid. After fully stirring, add 300mL of hot water, stir well, cover with surface III, heat in a water bath at 70-80℃ for 30min, cool, and filter with a G4 sand core crucible that has been dried to constant weight at 135±2℃. Rinse the insoluble matter in the beaker into the crucible with water. Wash until the washing liquid is colorless, then wash with 100mL of ammonia solution, wash with 10mL of hydrochloric acid solution, and then wash with water until the solution is free of white precipitate when detected by silver nitrate solution. Then put it in a constant temperature oven at 135±2℃ and bake it to constant weight.
4.5.3 Expression of analysis results
The mass percentage of insoluble matter in hydrochloric acid and ammonia water (X,) is calculated according to formula (3): X, = e × 100
Wherein: m2—mass of insoluble matter after drying, gm1——mass of sample?g.
4.5.4 Allowable difference
: The difference between the results of two parallel determinations shall not exceed 0.05%, and the arithmetic mean shall be taken as the determination result. 4.6 Determination of water-soluble chloride and sulfate content 4.6.1 Reagents and materials
Activated carbon;
Nitrobenzene (HG/T 3-903),
Nitric acid (GB/T626): (1+1) solution:
Silver nitrate (GB/T670): c(AgNO.)=0.1mol/L standard solution; d.
Ammonium thiocyanate (GB/T660): c(NH,CNS)=0.1mol/L standard solution; Ammonium ferric sulfate (GB/T1279) solution;
Preparation: Weigh 14 ml of ammonium ferric sulfate, dissolve it in 100 mL of water, filter, add 10 mL of nitric acid, and store in a brown bottle. 4.6.2 Preparation of sample solution
(3)
Weigh about 2 g of sample, accurate to 0.01 g, add 200.00 mL of water accurately, stir evenly, let stand for 30 min (stir continuously during this time), filter with dry filter paper. If the filtrate is colored, add 2 g of activated carbon and let stand for 1 h with occasional stirring, then filter with dry filter paper. If there is still color, replace the activated carbon and repeat the operation.
4.6.3 Determination of chloride content
4.6.3.1 Analysis steps
GB 6227.2--1995
Take 50mL of the above sample solution and place it in a 500mL conical flask. Add 2mL of nitric acid solution and 10mL of silver nitrate standard solution (add more when the chloride content is high) and 5mL of nitrobenzene. Shake vigorously until the silver chloride coagulates. Add 1mL of ammonium ferric sulfate test solution and titrate the excess silver nitrate with ammonium thiocyanate standard solution to the endpoint and keep for 1 min. At the same time, do a blank test in the same way. 4.6.3.2 Expression of analytical results
The mass percentage of chloride (X) shall be calculated according to formula (4): Xx - V.-V)·cX 0. 058 4 × 100 = (VV) :c×23.36%
Wherein: V -
the volume of 0.1 mol/L ammonium thiocyanate standard solution used to titrate the sample, mL; Ve
the volume of ammonium thiocyanate solution used to titrate the blank solution, mL; the concentration of the ammonium thiocyanate standard solution, mol/L: 0. 058 4 -
the mass of sodium chloride in grams equivalent to 1.00 mL of ammonium thiocyanate standard solution Cc (NH, CNS) = 1.000 mol/LJ,
the mass of the sample, nom.
4.6.3.3 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.3%, and the arithmetic mean shall be taken as the determination result. 4.6.4 Determination of sulfate (as sodium salt) content 4.6.4.1 Reagents and materials
Ammonia water (GB/T631);
Sodium hydroxide (GB/T629): 0.2g/L solution; Hydrochloric acid (GB/T622): (1+99) solution; Ethanol (GB/T679): 95%
Tetrahydroxybenzoic acid disodium-potassium chloride (GB/T646): Mix equal amounts of reagents; Sulfuric acid (GB/T625): c(1/2HzSO4)=0.1mal/L standard solution; Phenolic acid: 10g/L ethanol solution;
Rose Bengal Sodium acid indicator solution: weigh 0.1B of rose red sodium acid, dissolve in 10mL of water (prepare and use immediately); barium chloride (GB/T652): c(1/2BaCl.)=0.1mol/L standard solution; preparation: weigh 12.25g of barium chloride, dissolve in 500mL of distilled water, transfer to a 1000mL volumetric flask, dilute to the scale, shake well, calibration: absorb 20mL of sulfuric acid standard solution, add 50mL of water, and neutralize with ammonia water until bright yellow, the test paper shows alkaline reaction, then titrate with barium chloride standard solution, use rose red sodium acid indicator solution as external indicator, and the end point is the appearance of rose red spots on the filter paper that remain unchanged for 2min. The concentration of barium chloride standard solution (X:) is calculated according to formula (5): X,
where: V,—volume of sulfuric acid standard solution.mL; Vz volume of barium chloride standard solution, mL
c--—concentration of sulfuric acid standard titration solution, mol/L. 4.6.4.2 Analysis steps
GB 6227.21995
Pipette 25mL of the test solution and place it in a 250mL conical flask. Add 1 drop of phenolic acid indicator. Add sodium hydroxide solution until it turns pink. Then add hydrochloric acid solution until the pink disappears. Add 30mL of ethanol and 0.4g of tetrahydroxybenzene disodium and potassium chloride mixed indicator. Shake the spoon. After dissolving, titrate with sodium chloride standard solution under continuous shaking until the solution turns rose red. During the titration, use a light to illuminate from the side and observe carefully. Use sodium rose red acid indicator solution as an external indicator for comparison. At the same time, perform a blank test in the same way. 4.6.4.3 Expression of analysis results
The mass percentage of sodium sulfate (X.) is calculated according to formula (6): X. =- (VV) -c× 0. 071
(V1 - V) c X 56. 8
Wherein; V, — volume of barium chloride standard solution consumed in titrating the test solution, mL; V2 — volume of barium chloride standard solution consumed in titrating the blank solution, mL; c — actual concentration of monochlorinated standard solution, mol/L; X100
(6))
0.071 — mass of sodium sulfate expressed in grams equivalent to 1.00mL monochlorinated standard solution [c (1/2BaC12) = 1.000mol/L);
m — mass of the sample·g.
4.6.4.4 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. Note: The sum of the determination results of water-soluble chloride and sulfate content shall be less than or equal to 2%. 4.7 Determination of secondary dye content
4.7.1 Method summary
Use paper chromatography to separate and elute the components, and then quantify them by spectrophotometry. 4.7.2 Reagents and materials
Same as 4.7.2 of GB6227.1.
4.7.3 Instruments and equipment
Same as 4.7.3 of GB6227.1.
4.7.4 Paper chromatography conditions
Same as 4.7.4 of GB6227.1.
4.7.5 Analysis steps
Preparation of sample eluate: Weigh about 2g of the sample, accurate to Q.01g, place it in a beaker, add 80mL of water and 5g of sodium tartrate, heat to 90℃, stir to dissolve, transfer to a 100mL volumetric flask, dilute to the scale, and shake well. Use a micro-injector to accurately absorb 200μL of the above 2% solution, and evenly apply it on a baseline 25mm away from the bottom edge of the filter paper in a straight line, so that its width on the filter paper does not exceed 5mm and its length is 130mm. Use a hair dryer to blow dry, put the filter paper into the chromatography tank for development, and the bottom edge of the filter paper is thinned to 10mm below the liquid surface of the developing agent. When the front line of the developing agent rises to 150mm or until the secondary dye is separated satisfactorily, take it out and blow dry it with a hair dryer with cold air. At the same time, use a blank filter paper for development under the same conditions. The blank filter paper must be cut from the adjacent part of the same filter paper (.600mmX600mm>) as the filter paper used for developing the sample solution. Note: The chromatogram on the secondary dye paper is the same as GB6227.1. Cut the filter paper of each secondary dye and the corresponding part of the blank filter paper to the same size, place them in 50mL Nessler colorimetric tubes, accurately add 5mL of acetone solution, shake for 3~5min, then accurately add 20mL of sodium bicarbonate solution, shake thoroughly, filter the extracts naturally in No. 3 glass sand core funnels, pour the filtrate into a 50mm thick colorimetric III, and use a spectrophotometer to measure the absorbance at the maximum absorption wavelength of each secondary dye. Use 5mL of acetone solution and 20mL of sodium bicarbonate solution. The mixed solution is used as a reference solution. Preparation of standard sample eluate: Accurately pipette 6mL of the above 2% sample solution into a 100mL volumetric flask, dilute to the mark, and shake to hook. Use a micro-injector to draw 200 μL, evenly apply it on a baseline 25 mm from the bottom edge of the filter paper, wait until the front line of the developing agent rises only 40 mm, take it out and blow dry, cut off all the developed dye parts, extract the same operation as before, and measure the absorbance at the maximum absorption wavelength with a 10 mm colorimetric III. At the same time, use a blank filter paper to develop under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.6 Expression of analysis results The mass percentage of accessory dye (X,) shall be calculated according to formula (7): (A, -b) + +(A -bh)
(A. - B,)
the absorbance of each accessory dye extract calculated at a light path length of 50 mm; where: AA—
b1, bn——the absorbance of each accessory dye reference blank extract calculated at a light path length of 50 mm, A.
the absorbance of the standard reference blank extract calculated at a light path length of 10 mm, B.
——the absorbance of the standard reference blank extract calculated at a light path length of 10 mm; 5——the ratio converted to a light path length of 10 mm; 6——the reference concentration of the standard extract based on the 2% sample solution, %S——the total content of the sample.
4.7.7 Allowable differencewww.bzxz.net
The difference between the results of two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 4.8 Determination of arsenic content
(7)
The sample shall first be treated by the wet digestion method specified in 1.4.2.1 of GB8450, and then determined by the arsenic spot method specified in Method 2.
4.9 Determination of heavy metal content
4.9.1 Method summary
The sample shall be carbonized and ashed at high temperature, cooled, dissolved and filtered with acid, diluted to a certain volume, and sodium sulfide shall be added at pH = 4, and then limited colorimetry shall be performed.
Reagents and materials
Sulfuric acid (GB/T625);
Hydrochloric acid (GB/T 622);
Nitric acid (GB/T626)
Hydrochloric acid (GB/T622): (1+3) solution;
Ammonium acetate (GB/T1292): (1+9) solution, sodium sulfide (HG/T3-905): 100g/L solution Lead standard solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2.5g of the sample and put it into a porcelain pot, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it into an electric furnace and burn it at 450~550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, crush and grind thoroughly, evaporate to dryness on a water bath. Add 5mL of hydrochloric acid, crush and grind the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washing liquid, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washing liquid, adjust to pH 4 with ammonium acetate solution, add water to make up to 100mL, and use it as the sample solution. In addition, the same operation can be performed without adding the sample to use as the blank test solution. Take 40mL of the sample solution, add water to make up to 50mL, and use it as the detection solution. Take 40mL of blank test solution, add 2mL of lead standard solution, add water to make 50mL, as the comparison solution.
Add 2 drops of sodium sulfide test solution to each of the two solutions, shake well, and let stand for 5min. The color of the test solution should not be darker than that of the comparison solution. 4.10 Determination of lock content
4.10.1 Reagents and materials
Sulfuric acid (GB/T625):
Sulfuric acid (GB/T 625): (1+19) solution
Hydrochloric acid (GB/T622): (1+3) solution.
4.10.2 Analysis steps
Accurately weigh about 1g of the sample, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, and slowly heat it. Try to make it almost completely ash at a low temperature, then cool it, add 1mL of sulfuric acid, and slowly heat it until almost no sulfuric acid vapor is generated. Put it in an electric furnace and burn it at 450-550℃ for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix thoroughly, cover and heat to melt. Continue heating for 10 minutes, and after cooling, add 20.mL of water, heat on a water bath to dissolve the molten material. After cooling, filter, and wash the residue on the filter paper with water until the washing liquid does not react with sulfate. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake and mix thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10mL of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix. When left for 10 minutes, it should not be turbid. 5 Inspection rules
5.1 In the quality inspection of food additive sunset yellow aluminum lake, except for the content determination of lock, which is inspected at least once every quarter, the other? items are determined as factory inspection.
5.2 Except for each large box of 10×250g, the rest are the same as Article 5 of GB6227.1. 6 Marking, packaging, transportation, storage
6.1 Except for each small package of 250g, the rest are the same as Article 6 of GB6227.1. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard is drafted by Shanghai Dyestuff Research Institute and Shanghai Food Hygiene Supervision and Inspection Institute. The main drafters of this standard are Shi Huaimeng, Chen Qilong, Qian Kai, Qiu Yumei, Liu Jing and Yuan Yicheng. This standard is equivalent to the fifth edition of "Edible Yellow No. 5 Aluminum Lake" (Japanese Food Additive Code) in 1986. 4352%, and take the arithmetic mean as the determination result. 4.8 Determination of arsenic content
(7)
The sample is first treated by the wet digestion method specified in 1.4.2.1 of GB8450, and then determined by the arsenic spot method specified in Method 2.
4.9 Determination of heavy metal content
4.9.1 Method summary
The sample is carbonized and ashed at high temperature, cooled, dissolved and filtered with acid, diluted to a certain volume, and sodium sulfide is added at pH = 4, and then limited colorimetry is performed.
Reagents and materials
Sulfuric acid (GB/T625);
Hydrochloric acid (GB/T 622);
Nitric acid (GB/T626)
Hydrochloric acid (GB/T622): (1+3) solution;
Ammonium acetate (GB/T1292): (1+9) solution, sodium sulfide (HG/T3-905): 100g/L solution Lead standard solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2.5g of the sample and put it into a porcelain pot, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it into an electric furnace and burn it at 450~550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, crush and grind thoroughly, evaporate to dryness on a water bath. Add 5mL of hydrochloric acid, crush and grind the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washing liquid, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washing liquid, adjust to pH 4 with ammonium acetate solution, add water to make up to 100mL, and use it as the sample solution. In addition, the same operation can be performed without adding the sample to use as the blank test solution. Take 40mL of the sample solution, add water to make up to 50mL, and use it as the detection solution. Take 40mL of blank test solution, add 2mL of lead standard solution, add water to make 50mL, as the comparison solution.
Add 2 drops of sodium sulfide test solution to each of the two solutions, shake well, and let stand for 5min. The color of the test solution should not be darker than that of the comparison solution. 4.10 Determination of lock content
4.10.1 Reagents and materials
Sulfuric acid (GB/T625):
Sulfuric acid (GB/T 625): (1+19) solution
Hydrochloric acid (GB/T622): (1+3) solution.
4.10.2 Analysis steps
Accurately weigh about 1g of the sample, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, and slowly heat it. Try to make it almost completely ash at a low temperature, then cool it, add 1mL of sulfuric acid, and slowly heat it until almost no sulfuric acid vapor is generated. Put it in an electric furnace and burn it at 450-550℃ for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix thoroughly, cover and heat to melt. Continue heating for 10 minutes, and after cooling, add 20.mL of water, heat on a water bath to dissolve the molten material. After cooling, filter, and wash the residue on the filter paper with water until the washing liquid does not react with sulfate. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake and mix thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10mL of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix. When left for 10 minutes, it should not be turbid. 5 Inspection rules
5.1 In the quality inspection of food additive sunset yellow aluminum lake, except for the content determination of lock, which is inspected at least once every quarter, the other? items are determined as factory inspection.
5.2 Except for each large box of 10×250g, the rest are the same as Article 5 of GB6227.1. 6 Marking, packaging, transportation, storage
6.1 Except for each small package of 250g, the rest are the same as Article 6 of GB6227.1. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard is drafted by Shanghai Dyestuff Research Institute and Shanghai Food Hygiene Supervision and Inspection Institute. The main drafters of this standard are Shi Huaimeng, Chen Qilong, Qian Kai, Qiu Yumei, Liu Jing and Yuan Yicheng. This standard is equivalent to the fifth edition of "Edible Yellow No. 5 Aluminum Lake" (Japanese Food Additive Code) in 1986. 4352%, and take the arithmetic mean as the determination result. 4.8 Determination of arsenic content
(7)
The sample is first treated by the wet digestion method specified in 1.4.2.1 of GB8450, and then determined by the arsenic spot method specified in Method 2.
4.9 Determination of heavy metal content
4.9.1 Method summary
The sample is carbonized and ashed at high temperature, cooled, dissolved and filtered with acid, diluted to a certain volume, and sodium sulfide is added at pH = 4, and then limited colorimetry is performed.
Reagents and materials
Sulfuric acid (GB/T625);
Hydrochloric acid (GB/T 622);
Nitric acid (GB/T626)
Hydrochloric acid (GB/T622): (1+3) solution;
Ammonium acetate (GB/T1292): (1+9) solution, sodium sulfide (HG/T3-905): 100g/L solution Lead standard solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2.5g of the sample and put it into a porcelain pot, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it into an electric furnace and burn it at 450~550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, crush and grind thoroughly, evaporate to dryness on a water bath. Add 5mL of hydrochloric acid, crush and grind the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washing liquid, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washing liquid, adjust to pH 4 with ammonium acetate solution, add water to make up to 100mL, and use it as the sample solution. In addition, the same operation can be performed without adding the sample to use as the blank test solution. Take 40mL of the sample solution, add water to make up to 50mL, and use it as the detection solution. Take 40mL of blank test solution, add 2mL of lead standard solution, add water to make 50mL, as the comparison solution.
Add 2 drops of sodium sulfide test solution to each of the two solutions, shake well, and let stand for 5min. The color of the test solution should not be darker than that of the comparison solution. 4.10 Determination of lock content
4.10.1 Reagents and materials
Sulfuric acid (GB/T625):
Sulfuric acid (GB/T 625): (1+19) solution
Hydrochloric acid (GB/T622): (1+3) solution.
4.10.2 Analysis steps
Accurately weigh about 1g of the sample, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, and slowly heat it. Try to make it almost completely ash at a low temperature, then cool it, add 1mL of sulfuric acid, and slowly heat it until almost no sulfuric acid vapor is generated. Put it in an electric furnace and burn it at 450-550℃ for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix thoroughly, cover and heat to melt. Continue heating for 10 minutes, and after cooling, add 20.mL of water, heat on a water bath to dissolve the molten material. After cooling, filter, and wash the residue on the filter paper with water until the washing liquid does not react with sulfate. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake and mix thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10mL of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix. When left for 10 minutes, it should not be turbid. 5 Inspection rules
5.1 In the quality inspection of food additive sunset yellow aluminum lake, except for the content determination of lock, which is inspected at least once every quarter, the other? items are determined as factory inspection.
5.2 Except for each large box of 10×250g, the rest are the same as Article 5 of GB6227.1. 6 Marking, packaging, transportation, storage
6.1 Except for each small package of 250g, the rest are the same as Article 6 of GB6227.1. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard is drafted by Shanghai Dyestuff Research Institute and Shanghai Food Hygiene Supervision and Inspection Institute. The main drafters of this standard are Shi Huaimeng, Chen Qilong, Qian Kai, Qiu Yumei, Liu Jing and Yuan Yicheng. This standard is equivalent to the fifth edition of "Edible Yellow No. 5 Aluminum Lake" (Japanese Food Additive Code) in 1986. 4351, Article 6. Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai Dyestuff Research Institute and Shanghai Food Sanitation Supervision and Inspection Institute. The main drafters of this standard are Shi Huaimeng, Chen Qilong, Qian Kai, Qiu Yumei, Liu Jing and Yuan Yicheng. This standard is equivalent to the fifth edition of "Edible Yellow No. 5 Aluminum Lake" (Japanese Food Additive Code) in 1986. 4351, Article 6. Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai Dyestuff Research Institute and Shanghai Food Sanitation Supervision and Inspection Institute. The main drafters of this standard are Shi Huaimeng, Chen Qilong, Qian Kai, Qiu Yumei, Liu Jing and Yuan Yicheng. This standard is equivalent to the fifth edition of "Edible Yellow No. 5 Aluminum Lake" (Japanese Food Additive Code) in 1986. 435
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