Some standard content:
GB 4481.21999
This standard is equivalent to the 6th edition of the Japanese Food Additive Code (1992). GB4481.2-1994 is revised based on the standard "Edible Yellow No. 4 Aluminum Lake (Lemon Yellow Aluminum Lake)" in the book. The main technical differences between this standard and the Japanese standard are as follows: 1. The determination of secondary dyes continues to follow GB4481.2-1994, using the determination method in FAO/WHO, with an index of ≤0.5%, while the Japanese standard is the spot limit method.||t t||2. The determination method of arsenic (as As) content adopts the determination method of arsenic in food additives in GB/T8450-1987, and the index is ≤0.0003% (as As). The Japanese index is ≤0.0004% (As20). 3. In addition to the titanium trichloride titration method, a relatively simple spectrophotometric method is added for daily determination of product content. The titanium trichloride method is used as the arbitration method.
4. The determination method of oxide (as NaCl) and sulfate (as NazSO.) is Chemical titration method, Japanese standard is ion chromatography method, the main differences between this standard and GB4481.2-1994 are as follows: the test method of heavy metals (in terms of Pb), GB4481.2-1994 is atomic absorption spectrophotometry, this standard is limited colorimetric chemical analysis method.
This standard was first issued in 1994 and revised for the first time in 1999. From the date of implementation, this standard will replace GB4481.2-1994. This standard is issued by the State Petroleum and Chemical Industry This standard is under the jurisdiction of the National Dye Standardization Technical Committee and the Food Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by the Shanghai Dye Research Institute and the Health Supervision Institute of the Shanghai Municipal Health Bureau. The main drafters of this standard are Ding Deyi, Liu Jing, Shi Huaijiong, Ying Huiru, Guan Jianxiong, and Zhou Yanqin. This standard is entrusted to the National Dye Standard Technical Committee for interpretation. 391
National Standard of the People's Republic of China
Food Additives
Lemon Yellow Aluminum Lake
Food additive-
Tartrazine aluninum lake
GB 4481. 2 1999
Replaces GB4481.2—1994
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of the food additive tartrazine aluminum lake. This standard applies to the pigment lake formed by the reaction of food additive tartrazine with aluminum hydroxide. Molecular formula: CHN, O, S2
Relative molecular mass: 468.42 (according to the 1995 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T 6011988bzxZ.net
GB/T 602—1988
GB/T 603—1988
GB/T 6682—1992
GB/T 8450—1987
GB 4481. 1—1999
3.1 Appearance Yellow powder.
Chemical reagents
Chemical reagents
Preparation of standard solution for titration analysis (volumetric analysis) Preparation of standard solution for impurity determination
Chemical reagents Preparation of preparations and products used in test methods Specifications and test methods of water for analytical laboratories Determination of arsenic in food additives
Food additives Lemon yellow
3.2 The quality of the food additive lemon yellow aluminum lake shall meet the requirements of Table 1. Table 1 Requirements
Content (as color acid)
Loss on drying
Insoluble matter in hydrochloric acid and ammonia water
Chloride (as NaC) and sulfate (as NaSO,) Secondary dyes
Arsenic (as As)
Heavy metals (as Pb)
Barium (as Ba)
Approved by the State Administration of Quality and Technical Supervision on July 12, 1999 392
Implementation on January 1, 2000
4 Test methods
GB 4481. 2 -- 1999
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T6682. Unless otherwise specified, the standard solutions, impurity standard solutions, preparations and products required for the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
4.1 Appearance
Visual inspection.
4.2 Identification
4.2.1 Reagents and materials
a) Sulfuric acid;
b) Sulfuric acid solution: 1+20;
c) Hydrochloric acid solution: 1+3;
d) Ammonium acetate solution: 15g/L;
e) Sodium hydroxide solution: 100g/Lc
4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Test method
4.2.3.1 Weigh about 0.1g of sample, add 5mL of sulfuric acid, stir occasionally in a water bath, heat, and turn yellow in about 5min. After cooling, take 2-3 drops of the upper clear solution and add 5ml of water. It turns yellow. 4.2.3.2 Weigh about 0.1g of sample, add 5mL of sulfuric acid solution, heat in a water bath to dissolve, add ammonium acetate solution to 100mL, then absorb 2ml, and add ammonium acetate solution to 100mL. The maximum absorption wavelength of the solution should be 428nm ± 2nm. 4.2.3.3 Weigh about 0.1g of sample, add 10mL of hydrochloric acid solution, heat in a water bath to dissolve most of it, add 0.5g of activated carbon, shake well and filter. The solution is clear and turns yellow. Cool the solution and neutralize it with sodium hydroxide until a yellow colloidal precipitate gradually appears. 4.3 Determination of content
4.3.1 Titanium trichloride titration method (arbitration method)4.3.1.1 Summary of the method
In alkaline medium, the azo group in the dye is reduced and decomposed into amino compounds by titanium trichloride. The percentage of the dye content is calculated according to the consumption of titanium trichloride standard titration solution.
4.3.1.2 Reagents and materials
a) Trisodium citrate:
b) Sulfuric acid solution: 1+9;
c) Titanium trichloride standard titration solution: c (TiCl3a) = 0.1 mol/L (newly prepared, the preparation method is shown in Appendix A of GB4481.1-1999);
d) Carbon dioxide in cylinders.
4.3.1.3 Analysis steps
Weigh about 7g of sample, accurate to 0.0002g, add 80mL of sulfuric acid solution, stir and dissolve at 40℃～50℃, transfer to a 20ml volumetric flask, dilute to the scale with freshly boiled water that has been cooled to room temperature, shake well, pipette 50mL, place in a 500mL conical flask, add 30g of trisodium citrate and 200mL of water, assemble the instrument as shown in Figure 1, heat to boiling while passing a stream of carbon dioxide under the liquid surface, and titrate with titanium trifluoride standard titration solution until the colorless end point. 393
1-conical flask (500ml); 2-brown burette (50ml); 3-glass bottle with a black paper bottom (2000ml): 1-container for a mixture of 10% ammonium carbonate and 10% ferrous sulfate (5000ml); 5-piston: 6-empty bottle; 7-wash bottle with water
Figure 1 Apparatus diagram for titanium trichloride titration
4.3.1.4 Expression of analytical results
The content of lemon yellow aluminum lake (X) expressed in mass percentage is calculated according to formula (1): -V×c×0.1171 × 100 = Y×cX 58.55X.=
m×250
Wherein 1: V-the volume of the titanium trichloride standard titration solution consumed for titration of the sample + mL: ---the actual concentration of the titanium trichloride standard titration solution + mol/L; the mass of the sample, g;
0. 117 1-
the mass of the lemon yellow aluminum lake expressed in grams equivalent to 1.00mL of the titanium trichloride standard titration solution [c(TiCl:)=1mol/L] + g.
4.3.1.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%, and the arithmetic mean shall be taken as the determination result. 4.3.2 Spectrophotometric colorimetric method
4.3.2.1 Summary of the method
After the sample and the standard sample with known content are dissolved in water respectively, their absorbances are measured at the maximum absorption wavelength respectively, and then the content of the sample is calculated.
4.3.2.2 Reagents and materials
a) Sodium hydrogen tartrate;
b) Tartrazine standard: ≥85.0%: content is determined by titration with titanium trifluoride. 4.3.2.3 Instruments and equipment
a) Spectrophotometer;
h) Colorimetric III: 10mm.
4.3.2.4 Preparation of lemon yellow standard solution
Weigh more than 0.5g of lemon yellow standard sample, accurately to 0.0002g, dissolve in an appropriate amount of water, transfer to a 1000mL volumetric flask, dilute to the scale, and shake well. Accurately draw 10mL, transfer to a 500ml volumetric flask, dilute to the scale, and shake well. .394
4.3.2.5 Preparation of lemon yellow aluminum lake sample GB 4481. 2 - 1999
Weigh 4.25g of lemon yellow aluminum lake sample, accurate to 0.0002g, add 20mL of water and about 2g of sodium hydrogen tartrate, and slowly heat to 90°C. The rest is the same as the preparation of lemon yellow standard solution. 4.3.2.6 Test method
Measure the absorbance of the standard solution and the sample solution at a wavelength of 428nm±2nm on a spectrophotometer using 10mm colorimetric blood.
Use water as the reference solution.
4.3.2.7 Expression of analysis results
The content of lemon yellow aluminum lake expressed as mass percentage (X,) is calculated according to formula (2): X
Where: A--absorbance of test solution;
A.--absorbance of standard solution:||tt ||×x×10
X. 一—Mass percentage of standard sample of lemon yellow aluminum lake (titanium chloride method); 10/85—Total content of sample:
4.3.2.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 2.0%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of drying loss content
According to 4.4.1 of GB4481.1-1999. 4.5 Determination of insoluble matter content in hydrochloric acid and ammonia water 4.5.1 Reagents and materials
a) Hydrochloric acid;
b) Hydrochloric acid solution: 3+7;
c) Ammonia solution: 4+96;
d) Silver nitrate solution: c(AgNO,)=o.1mol/L. 4.5.2 Test method
Weigh about 2g of sample, accurate to 0.01g, put it in a 600mL beaker, add 20mL of water and 20mL of hydrochloric acid. After fully stirring, add 300mL of hot water, stir well, and cover the surface with blood. 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 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 has no white precipitation when detected by silver nitrate solution, then put it in a weighing bottle dried to constant weight in a constant temperature oven at 135℃±2℃, and bake in a constant temperature oven at 135℃±2℃ to constant weight. . 4.5.3 Expression of analysis results
Express the insoluble matter content (X,) in hydrochloric acid and ammonia water in mass percentage and calculate it according to formula (3): mi×100
Where: m,-
Mass of insoluble matter after drying, name;
-Mass of sample g.
4.5.4 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.10%, and the arithmetic mean shall be taken as the determination result. 4.6 Chloride (NaCl The determination of chloride (calculated as NaCl) and sulfate (calculated as Na2SO4) content shall be carried out in accordance with GB4481.1-1999 4.4.2 and 4.4.3. The total mass percentage of chloride (calculated as NaCl) and sulfate (calculated as NazSO4) shall not exceed 2.0%. 4.7 Determination of secondary dye content
4.7.1 Reagents and materials
a) Anhydrous ethanol;
b) n-butanol;
() Acetone solution: 1+1;
d) Ammonia solution: 4+96;
e) Sodium bicarbonate solution: 4g/L;
f) Sodium hydrogen tartrate.
4.7.2 Instruments and equipment
a) Spectrophotometer;
GB 4481. 2 - 1999
h) Chromatographic filter paper: No. 1 medium speed, 150mm×250mm;c) Chromatographic cylinder: $240mmX300mm;
d) Micro-injector: 100μL.
4.7.3 Analysis steps
4.7.3.1 Paper chromatography conditions
a) Developing solvent: n-butanol + anhydrous ethanol + ammonia solution = 6 + 2 + 3. b) Temperature: 20℃～25℃.
4.7.3.2 Preparation of sample eluate
Weigh about 2g of sample, accurate to 0.01g, place in a beaker, add 80mL of water and 6g of sodium hydrogen tartrate, slowly heat to 90℃, stir to dissolve, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Use a microinjector to accurately draw 200μL, 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. Blow it dry with a hair dryer, put the filter paper in the chromatography tank for development, immerse the bottom edge of the filter paper 10mm below the liquid surface of the developing agent, wait until the front line of the developing agent rises to 15mm or until the secondary dye is separated satisfactorily (see Figure 2), take it out, and blow it dry 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 600nmX600mm filter paper as the filter paper used for developing the sample solution. 150mm
Secondary dye
Main dye
Figure 2 Schematic diagram of secondary dye on-paper chromatography
GB 4481. 2-1999
Cut the secondary dye and the filter paper corresponding to the secondary dye on the blank filter paper into the same size, and cut into 5mm×15mm thin strips, put them in a 50mL Nessler colorimetric tube, accurately add 5mL of acetone solution, shake for 3min~5min, then add 20mL of sodium bicarbonate solution, shake thoroughly, and filter the extracts naturally in No. 3 glass sand core funnels. The filtrate must be clear and free of suspended matter. Use a 50mm colorimetric dish to measure the absorbance at the maximum absorption wavelength of the secondary dye. Use a mixture of 5mL acetone solution and 20mL sodium bicarbonate solution as the reference solution. 4.7.3.3 Preparation of standard eluate
Accurately pipette 6mL of the above 2% sample solution into a 100mL volumetric flask, dilute to the mark, and spread. Use a microinjector to pipette 200μl and evenly apply it on a baseline 25mm away from the bottom edge of the filter paper. Blow it dry with cold air, place the filter paper in the chromatography tank and develop it. When the front line of the developing agent rises only 40mm, take it out and blow it dry. For all the dye parts cut off, perform the extraction operation as before, and measure the absorbance at the maximum absorption wavelength with a 10mm colorimetric dish.
At the same time, develop with blank filter paper under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.4 Expression of analysis results
Express the content of lemon yellow aluminum lake secondary dye (X4) in mass percentage and calculate it according to formula (4): A-6
X4= A b.
Wherein: A is the absorbance of the secondary dye extract calculated at a light path length of 50 mm; b is the absorbance of the secondary dye reference blank extract calculated at a light path length of 50 mm; A is the absorbance of the standard extract calculated at a light path length of 10 mm; b is the absorbance of the standard reference blank extract calculated at a light path length of 10 mm; 5 is the ratio converted to a light path length of 10 mm; 6 is the reference concentration of the standard extract based on the 2% sample solution, %; 10
The total content of the sample.
4.7.5 Allowable difference
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
According to 4.7 of GB4481.1-1999.
4.9 Determination of heavy metal content
4.9.1 Reagents and materials
a) Sulfuric acid:
b) Hydrochloric acid;
c) Nitric acid;
d) Hydrochloric acid solution: 1+3;
e) Ammonium acetate solution: 1+9;
(4)
f) Sodium sulfide solution: 100g/L;
g) Lead standard solution: 0.01mg/ml. Take 10mL of the lead standard solution containing 0.1mg/mL of lead (Pb) in a 100mL volumetric flask and dilute to the scale.
4.9.2 Test method
Weigh 2.5g of the sample to an accuracy of 0.0.1g, put it in a quartz or porcelain tower, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, let it cool, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace, burn it at 450℃~550C for 3h, and let it cool. Add 5mL of hydrochloric acid and 1mL of nitric acid, crush it thoroughly, evaporate it to dryness on a water bath. Add 5ml of hydrochloric acid, crush the block thoroughly, evaporate it to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool it, and filter it with quantitative analysis filter paper (No. 5C). Wash the residue on the filter paper with 30mL of hydrochloric acid solution, combine the washing liquid and the filtrate, and evaporate it to dryness on a water bath. Add 10 ml of hydrochloric acid solution 397
GB 44812—1999
to the residue, heat to dissolve, filter after cooling, and then wash the residue on the container and filter paper with 5 ml of hydrochloric acid solution and 5 ml of water. Combine the washing liquid and the filtrate, add water to 50 ml, and use it as the sample solution. Perform the same operation without the sample as the blank test solution. Measure 20 ml of the sample solution, add ammonium acetate solution, adjust to a pH value of about 4, and add water to 50 ml as the test solution. Separately measure 20 ml of the blank test solution and 2.0 ml of the lead standard push solution, and operate in the same way as the sample to prepare the comparison solution. Add 2 drops of sodium sulfide test solution to each of the two solutions, shake well, and let stand for 5 minutes. The color of the test solution should not be darker than that of the comparison solution. 4.10 Determination of barium content
4.10.1 Reagents and materials
a) Sulfuric acid;
b) Sulfuric acid solution: 1+19;
c) Hydrochloric acid solution: 1→3.
4.10.2 Test method
Accurately weigh 1g of the sample, accurate to 0.01g, put it in a platinum (porcelain or quartz) bowl, add a small amount of sulfuric acid to moisten it, slowly heat it, try to make it almost completely ash at a low temperature, let it cool, add 1mL of sulfuric acid, slowly heat 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 10min, cool it, add 20mL of water, heat it on a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not show sulfate reaction. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake 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 placed for 10 minutes, it shall not be turbid.
5 Inspection rules
5.1 The quality inspection department of the production unit shall inspect the product quality of the food additive lemon yellow aluminum lake in accordance with the provisions of this standard. The production unit shall ensure that the quality of all food additives lemon yellow aluminum lakes shipped out of the factory meets the requirements of this standard and have a quality certificate in a certain format.
5.2 The food additive lemon yellow aluminum lake is a batch of uniform products mixed once. 5.3 For bottled products, 10% of the total number of product packaging boxes (each box is 10×150g) in each batch should be selected for sampling, and then 10% of the bottles should be selected from the selected boxes. From the selected bottles, take out no less than 50g of samples from the center of each bottle. Be careful when sampling to prevent foreign impurities from falling into the product. Mix the collected samples quickly and take about 100g from them. Put them in two clean and dry ground-mouth glass bottles, seal them with paraffin, and label them with the manufacturer name, product name, batch number, and sampling date. One bottle is for inspection and the other bottle is kept for future reference. 5.4 If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for re-inspection. If one of the indicators in the re-inspection results still does not meet the requirements of this standard, the batch of products is unqualified. 5.5 The user has the right to accept the quality of the food additive lemon yellow lead lake received in accordance with the inspection rules and test methods specified in this standard.
6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box should have firm and clear markings, including the words "food additive colorant", product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, and shelf life. 6.2 Each bottle of product leaving the factory should have a clear mark, including the words "food additive", product name, manufacturer name and address, trademark, production and food hygiene license number, product standard number and standard name, shelf life, production date and batch number, net content, and instructions for use. 6.3 The food additive lemon yellow aluminum lake is packed in polyethylene plastic bottles, 150g per bottle, and every 10 bottles are sealed in an outer box. Other forms of packaging can be determined by negotiation between the manufacturer and the user.
6.4 It must be protected from rain, moisture, and sunlight during transportation, and should be stored in a dry and cool warehouse. 398
GB4481.21999
This product must not be mixed, transported or stacked with other toxic or harmful substances during storage and transportation. 6.5
5 The shelf life of this product is five years from the date of production. It can only be used after re-inspection and in full compliance with the requirements of this standard. 6.61. The packaging box should have firm and clear markings, including the words "food additive colorant", product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, and shelf life. 6.2. Each bottle of product leaving the factory should have a clear mark, including the words "food additive", product name, manufacturer name and address, trademark, production and food hygiene license number, product standard number and standard name, shelf life, production date and batch number, net content, and instructions for use. 6.3. The food additive lemon yellow aluminum lake is packed in polyethylene plastic bottles, 150g per bottle, and sealed in outer boxes for every 10 bottles. Other forms of packaging can be determined by negotiation between the manufacturer and the user.
6.4. It must be protected from rain, moisture, and sunlight during transportation, and should be stored in a dry and cool warehouse. 398
GB4481.21999
This product must not be mixed, transported, or stacked with other toxic or harmful substances during storage and transportation. 6.5
5The shelf life of this product is five years from the date of production. It can only be used after re-inspection and full compliance with the requirements of this standard.1. The packaging box should have firm and clear markings, including the words "food additive colorant", product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, and shelf life. 6.2. Each bottle of product leaving the factory should have a clear mark, including the words "food additive", product name, manufacturer name and address, trademark, production and food hygiene license number, product standard number and standard name, shelf life, production date and batch number, net content, and instructions for use. 6.3. The food additive lemon yellow aluminum lake is packed in polyethylene plastic bottles, 150g per bottle, and sealed in outer boxes for every 10 bottles. Other forms of packaging can be determined by negotiation between the manufacturer and the user.
6.4. It must be protected from rain, moisture, and sunlight during transportation, and should be stored in a dry and cool warehouse. 398
GB4481.21999
This product must not be mixed, transported, or stacked with other toxic or harmful substances during storage and transportation. 6.5
5The shelf life of this product is five years from the date of production. It can only be used after re-inspection and full compliance with the requirements of this standard.
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