Some standard content:
GB 17511. 2--1998
This standard is equivalent to the "Japanese Food Lacquer Additives (1992 Sixth Edition)", and is formulated based on the standard of edible red 40 aluminum lake (tempting red aluminum lake) in the book. The differences between this standard and the Japanese standard are as follows:
1. In addition to the titanium trichloride titration method, the spectrophotometry method is added to the product content determination in this standard. This method is used as the daily determination method, and the titanium trichloride method is used as the arbitration method.
2. The determination method of chloride (in terms of NaCl) and sulfate (in terms of NazSO) in this standard is chemical titration, while the Japanese standard is ion chromatography. wwW.bzxz.Net
3. The determination method of the content of ascorbyl in this standard adopts GB/T8450--1987 "Determination of ascorbyl in food additives", and the index is ≤0.0003% (As). The Japanese index is ≤0.0004% (As20). This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is drafted by the former dye standardization and promotion technical unit of the Ministry of Chemical Industry and the Food Supervision and Inspection Institute of the Ministry of Health. This standard is drafted by the Shanghai Dyestuff Research Institute and the Shanghai Industrial and Health Bureau Health Supervision Institute. The main drafters of this standard are Ding Deyi, Di Jinjun, Bang Guo, Ying Huiru, Shi Huaimeng and Zhou Yanqin. This standard is entrusted to the former dye standardization and promotion technical unit of the Ministry of Chemical Industry for interpretation. 533
National Standard of the People's Republic of China
Food additive
Fancy (Allura) red aluminum lake
Food additive
Fancy (Allura) red aluminum lakeGB17511. 2—1998
This standard specifies the requirements, test methods, inspection rules, marking, packaging, transportation and storage of the food additive Fancy (Allura) red aluminum lake. This standard applies to the pigment lake formed by the reaction of the food additive allura red with aluminum hydroxide. This product can be added to food as a colorant.
Molecular formula: CHN, O, S2
Relative molecular mass: 452.46 (according to the 1995 International Relative Atomic Mass) 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. All parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601--1988 Chemical reagents - Preparation of standard solutions for titration analysis (volumetric analysis) GB/T602—1988 Chemical reagents
Preparation of standard solutions for impurity determination
GB/T603--1988 Chemical reagents
Preparation of preparations and products used in test methods Specifications and test methods for water for analytical laboratories (negISO3696:1987) GB/T6682-1992
GB 17511. 1—1998
3 Requirements
3.1 Appearance: red powder.
Food additives attractant red
3.2 Food additives attractant red aluminum lake shall meet the requirements of Table 1: Table 1 requirements
Content (in terms of color acid)
Loss on drying
Chloride (in terms of NaCl)
And sulfate (in terms of NazSO.)
Insoluble matter in hydrochloric acid and ammonia water
Low sulfonated secondary dye
High sulfonated secondary dye
Approved by the State Administration of Quality and Technical Supervision on October 19, 1998 53-1
Implemented on April 1, 1999
G 17511.2-1998
Table 1 (end)
6-Hydroxy-5-1-(2-methoxy-5-methyl-4-sulfonylbenzene)azo-8-(2-methoxy-5-methylsulfonylphenoxy)-2-naphthalenesulfonic acid disodium salt
6-Hydroxy-2-naphthalenesulfonic acid sodium salt
4-Amino-5-methoxy-2-methylbenzenesulfonic acid 6,6-oxo-bis(2-naphthalenesulfonic acid) disodium salt
Unsulfonated aromatic primary amines (calculated as aniline)
Monochromic acid (As)
Heavy metals (calculated as Pbh)
Lead (Pb)
Barium (Ba)
4 Test methods
The reagents and water used in this standard are not When other requirements are specified, they refer to analytical pure reagents and grade 3 water specified in GB/TB682. 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 when no other requirements are specified.
4-1 Appearance
Measured by visual inspection.
4.2 Identification
4.2.1 Reagents and materials
) Sulfuric acid;
b) Sulfuric acid solution: 1+20
r) Ammonium acetate solution: 1.5g/L;
d) Hydrochloric acid solution: 1+3
e) Sodium hydroxide solution: 90g/L;
1 Activated carbon.
4.2.2 Apparatus and equipment only
Spectrophotometer.
4.2.3 Test method
4.2.3.1 Weigh 0.1g sample, add 5mL vegetable acid, shake and heat in a water bath from time to time, the solution turns dark purple-red for about 5 minutes, cool, take 2-3 drops of the upper clear liquid, add 5mL water, the solution turns red. 4.2.3.2 Weigh 0.1g sample, add 5mL sulfuric acid solution, shake well, add ammonium acetate solution to 100mL, centrifuge when the solution is turbid, then measure 1-10ml of this solution, add acetic acid solution to 100mL, and measure the absorbance (within the range of 0.2-0.7), the maximum absorption peak is at a wavelength of 499nm ± 2nm. 4.2.3.3 Weigh 0.1g sample, add 10mL hydrochloric acid solution, heat in a water bath to dissolve most of it, add 0.5 more activated carbon, shake well, filter, take the colorless filtrate, add sodium hydroxide solution, and react with the resulting liquid to show salt. 4.3 Determination of Allura Red Aluminum Lake Content
4.3.1 Titanium trichloride titration method (arbitration method) 4.3.1.1 Method Summary
In alkaline medium, the azo group in the dye is reduced and decomposed into amino compounds by titanium trifluoride. The percentage content of the dye is calculated according to the consumption of 533% of titanium trichloride standard solution.
4.3.7.2 Reagents and materials
a) Trisodium citrate:
b) Sulfuric acid solution: 1+9;
GB 17511. 2- 1998
c) Titanium trichloride standard solution: c(TiCl:)=0.1mol/L, freshly prepared. The preparation method is shown in Appendix A of GB17511.1-1998; d) Carbon dioxide in cylinders.
4.3.1.3 Analysis steps
Weigh 7g of sample, accurate to 0.0002g. Add 80mL of sulfuric acid solution, stir and dissolve at 40-50℃, transfer to a 250mL volumetric flask, dilute to scale with freshly boiled water that has been cooled to room temperature, accurately draw 50mL with a hook, place in a 500mL conical flask, add 30g of trisodium citrate and 200mL of water. Assemble the instrument as shown in Figure 1 of GB17511.1-1998, 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. The mass percentage X of the allure red aluminum lake is calculated according to the formula (1): Vc×0.1131×100
m×250
Wherein: V is the volume of the titanium trichloride standard solution consumed for titrating the sample, mL; c is the actual concentration of the titanium trichloride standard solution, mol/L1);
0.1131~ is the mass of the allure red aluminum lake in grams equivalent to 1.00mL of the titanium trichloride standard titration solution [c(TiCl,)=1.000mol/L];
The mass of the sample, g.
4.3.1.4 Allowable difference
The difference between the results of two parallel determinations shall not be less than 1%, and the arithmetic mean shall be taken as the determination result. 4.3.2 Spectrophotometric colorimetry
4.3.2.1 Method summary
After preparing solutions of the sample and the standard sample with known content, measure their absorbance at the maximum absorption wavelength, and then calculate the content of the sample.
4.3.2.2 Reagents and materials
a) Ammonium acetate solution: 1.5g/L;
b) Sulfuric acid solution: 1+20.
4.3.2.3 Instruments and equipment
a) Spectrophotometer;
b) Cuvette: 10mm.
4.3.2.4 Preparation of the standard sample solution of the allure red aluminum lake Weigh 0.5g of the standard sample of the allure red aluminum lake, accurate to 0.0002g. Add 25mL of sulfuric acid solution, shake well, and add ammonium acetate solution to 1000mL. When the solution is turbid, centrifuge and separate. Then take 10mL of this solution and add ammonium acetate solution to 500mL. 4.3.2.5 Preparation of Allure Red Aluminum Lake Sample Solution The weighing and operation methods are the same as those for the preparation of the standard solution. 4.3.2.6 Test Method
Put the standard solution and the test solution in a 10mm colorimetric III and measure their absorbances at a wavelength of 499nm±2nm using a spectrophotometer.
Use ammonium acetate solution as the reference solution.
4.3.2.7 Expression of analysis results
The mass percentage of Allura Red Aluminum Lake X is calculated according to formula (2): 536
Wherein: A——absorbance of test solution: A.—absorbance of standard solution;
GB 17511. 2 -- 1998
X, —-mass percentage of Allura Red Aluminum Lake standard sample (titanium chloride method). 4.3.2.8 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. 4.4 Determination of loss on drying
Perform according to 4.4.1 of GB17511.1-1998. 4.5 The determination of chloride (as NaCl) and sulfate (as NazSO.) content shall be carried out in accordance with 4.4.2~4.4.3 of GB17511.1-1998. (2)
The sum of the mass percentage of chloride (as NaCl) and sulfate (as Na,SO.) shall not exceed 2.0%.
4.6 Determination of insoluble matter content in hydrochloric acid and ammonia water 4.6.1 Reagents and materials
a) Hydrochloric acid;
b) Hydrochloric acid solution: 3+7:
c) Ammonia solution: 4+96:
d) Silver nitrate solution: c(AgNO.)=0.1mol/L. 4.6.2 Analysis steps
Weigh 2g of sample to an accuracy of 0.001g. Place in a 600mL beaker, add 20mL of water and 20mL of concentrated hydrochloric acid, stir thoroughly, add 300mL of hot water, stir well, cover with a watch glass, heat in a water bath at 70~80℃ for 30min, and let cool. Filter with G4 glass sand 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, first wash with 100mL of ammonia solution, then wash with 10mL of hydrochloric acid solution, and then wash with water until there is no white precipitation detected by silver nitrate solution, then place in a constant temperature oven at 135℃±2℃ and dry to constant weight.
4.6.3 Expression of analysis results
The mass percentage X of insoluble matter in hydrochloric acid and ammonia water is calculated according to formula (3): ml×100
Where; m1--the mass of insoluble matter after drying, g; - the mass of the sample·g.
4.6.4 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. 4.7 Determination of low sulfonated secondary dye content
4.7.1 Reagents and materials
a) Ammonium acetate solution: 7.8g/l
b) Sulfuric acid solution: 1+20.
4.7.2 Instruments
Liquid chromatograph.
4.7.3 Preparation of test solution
Weigh 0.1g of the sample, accurate to 0.0002g. Add 5mL of sulfuric acid solution, shake well, then add 130mL of ammonium acetate solution. When the solution is turbid, centrifuge and separate it, and use this solution as the test solution. 4.7.4 Test method
GB 17511. 2 1998
Measure 20μL of the test solution in 4.7.3. The following shall be carried out in accordance with 4.6.4~4.6.6 of GB17511.1--1998. 4.8 Determination of high sulfonated dye content
4.8.1 Reagents and materials
Same as 4.7.1.
4.8.2 Instrument
Same as 4.7.2.
4.8.3 Test method
Measure 20μL of the test solution in 4.7.3. The following shall be carried out in accordance with 4.7.4~4.7.6 of GB17511.1--1998. 4.9 Determination of 6-hydroxy-5-[(2-methoxy-5-methyl-4-sulfonylbenzene)azo}-8-(2-methoxy-5-methyl-4-sulfonylphenoxy)-2-naphthalenesulfonic acid disodium salt
4.9.1 Reagents and materials
Same as 4.7.1.
4.9.2 Instrument
Same as 4.7.2.
4.9.3 Test method
Measure 20#L of the test solution in 4.7.3. The following is carried out in accordance with 4.8.4~4.8.6 of GB17511.1-1998. 4.10 Determination of 6-hydroxy-2-naphthalenesulfonic acid sodium content4.10.1 Reagents and materials
Same as 4.7.1.
4.10.2 Instrument
Same as 4.7.2.
4.10.3 Test method
Measure 20μL of the test solution in 4.7.3. The following shall be carried out in accordance with 4.9.4~4.9.6 of GB17511.1-1998. 4.11 Determination of 4-amino-5-methoxy-2-methylbenzenesulfonic acid content 4.11.1 Reagents and materials
Same as 4.7.1.
4.11.2 Instrument
Same as 4.7.2.
4.11.3 Test method
Measure 20μL of the test solution in 4.7.3. The following shall be carried out in accordance with 4.10.4~4.10.6 of GB17511.1-1998. 4.12 Determination of the content of 6,6°-oxo-bis(2-naphthalenesulfonic acid) disodium salt 4.12.1 Reagents and materials
Same as 4.7.1.
4.12.2 Instrument
Same as 4.7.2.
4.12.3 Test method
Measure 20 μL of the test solution in 4.7.3. The following shall be carried out in accordance with 4.11.4 to 4.11.6 of GB17511.1-1998. 4.13 Determination of the total content of unsulfonated aromatic primary amines (calculated as aniline) 4.13.1 Reagents and materials
Same as 4.12.1 of GB17511.1-1998.
4.13.2 Instrument
Same as 4.12.2 of GB17511.1-1998.
4.13.3 Preparation of test solution
GB 17511. 2-1998
Weigh 5.0g of the sample, accurate to 0.0002g, add 70mL of chloroform, shake well from time to time and let stand for 1h, filter with dry quantitative analysis filter paper (No. 5C), collect the filtrate into a 200mL round-bottom flask, wash the residue on the filter paper with 10ml of chloroform 3 times, combine the washing liquid and the filtrate, add 5mL of sulfuric acid (0.15+1000) solution as the test solution. 4.13.4 Test method
Perform according to 4.12.4~4.12.6 of GB17511.1-1998. 4.14 Determination of arsenic content
Perform according to 4.13 of GB17511.1-1998. 4.15 Determination of heavy metal content
4.15.1 Reagents and materials
a) Sulfuric acid;
b) Hydrochloric acid;
c) Nitric acid;
d) Hydrochloric acid solution: 1+3;
e) Ammonium acetate solution: 1+9;
1) Sodium sulfide solution: 100g/L:
g) Lead standard solution: 0.01mgPb/mL. Take 10mL of the lead standard solution containing 0.1mgPb/mL in a 100mL volumetric flask and dilute to the scale.
4.15.2 Preparation of sample solution
Weigh 2.5g of the sample to an accuracy of 0.01g. Put it in a quartz or porcelain crucible, add a little sulfuric acid to moisten it, slowly burn it, and try to ash it at low temperature, then cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace and burn it at 450~~550C for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, crush it thoroughly, and evaporate it to dryness on a water bath. Add 5mL of hydrochloric acid, crush the block thoroughly, and evaporate it to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, and filter it with quantitative analysis filter paper (No. 5C) after cooling. Wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washing liquid, evaporate it to dryness on a water bath, and add 10mL of hydrochloric acid solution to heat to dissolve. After cooling, filter it. Then wash the container and the residue on the filter paper with 5mL of hydrochloric acid solution and 5mL of water, combine the washing solution and the filtrate, add water to make up to 50mL as the sample solution.
In addition, perform the same operation without adding the sample to serve as the blank test solution. 4.15.3 Preparation of test solution
Pipette 20 mL of the sample solution into a Nessler colorimetric tube, add ammonium acetate solution to adjust the pH value to about 4, and then add water to make it 50 mL as the test solution.
4.15.4 Preparation of comparison solution
In addition, measure 20 mL of blank test solution and 2.0 mL of lead standard solution into a Nessler colorimetric tube and perform the same operation as the test solution to make the comparison solution. 4.15.5 Test method
Add 2 drops of sodium sulfide test solution to the test solution and the comparison solution respectively, shake well, and let stand for 5 minutes. The color of the test solution should not be darker than that of the comparison solution. 4.16 Determination of lead content
4.16.1 Reagents and materials
Same as 4.15.1.
4.16.2 Preparation of test solution
Pipette 10 mL of the sample solution in 4.15.2 as the test solution. 4.16.3 Preparation of comparative solution
Pipette 1.0mL of lead standard solution and add hydrochloric acid solution to prepare 20mL as comparative solution. 4.16.4 Test method
Add 2 drops of sodium sulfide test solution to the test solution and comparative solution respectively, shake well, and let stand for 5 minutes. The color of the test solution should not be darker than that of the comparative solution. 4.17 Determination of content
4.17.1 Reagents and materials
a) Sulfuric acid;
b) Sulfuric acid solution: 1+19;
c) Hydrochloric acid solution: 1+3.
4.17.2 Analysis steps
GB17511.2-1998
Weigh about 1g of the sample, accurate to 0.01g. Place in a platinum (quartz or porcelain) crucible, add a small amount of sulfuric acid to moisten, slowly heat, try to make it almost completely ash at low temperature, let it cool, add 1mL of sulfuric acid, and slowly heat until almost no sulfuric acid vapor is generated. Place in an electric furnace, burn at 450~550C for 3h, cool, add 5g of anhydrous sodium carbonate and mix thoroughly, cover and heat to melt. Continue heating for 10min, cool, add 20mL of water, heat 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 react with sulfate. Then move the residue on the paper and the filter paper to a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. Cool, filter, wash the residue on the filter paper with 10mL of water, combine the washing liquid with the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to make it 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 tempting red aluminum lake, the content determination is type inspection, which is sampled once every quarter, and other items are factory inspection.
5.2 Food additive tempting red aluminum lake should be inspected by the product quality inspection department of the production unit. The production unit should ensure that the quality of all food additive tempting red lead lakes shipped from the factory meets the requirements of this standard and have a quality certificate in a certain format. 5.3 The user can inspect the quality of the food additive tempting red aluminum lake received in accordance with the inspection rules and test methods specified in this standard to check whether its quality indicators meet the requirements of this standard. 5.4 Food additive tempting red aluminum lake is a batch of products with one production batch number. 5.5 Sampling should be done by selecting 10% of the total number of boxes (each box is 10×0.15kg) of each batch of product packaging boxes, and then selecting 10% of the bottles from the selected boxes. From the selected bottles, take out samples of no less than 50g at the center of each bottle. Be careful when taking samples to prevent foreign matter from falling into the product. Mix the samples quickly and take about 100 of them, and put them in two clean, dry ground-mouth glass bottles, and seal them with paraffin wax, and indicate the manufacturer name, product name, batch number, and production date. One bottle is for inspection and one bottle is for storage. 5.6 If one of the indicators in the inspection does not meet the requirements of this standard, samples should be selected from twice the amount of packaging for re-inspection. If the result of the re-inspection still does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have obvious markings, including: "food additives", product name, trademark, manufacturer name, manufacturer address, specifications, batch number, production date, production license number, number of bottles. 6.2 Each bottle of product leaving the factory should be accompanied by a quality certificate, including: manufacturer name, product name, batch number, production date, net content, usage, shelf life, proof that the product quality meets this standard and standard number. 6.3 Food additive temptation red aluminum lake is packed in polyethylene plastic bottles, 0.15kg per bottle, and every 10 bottles are sealed in an outer box. 6.4 It must be protected from rain, moisture and sunlight during transportation. It should be stored in a dry and cool warehouse. 6.5 This product must not be mixed, transported or stacked together with other toxic and harmful substances during storage and transportation. 6.6 The shelf life of this product is five years from the date of production. Re-inspect whether it meets the requirements of this standard after the expiration date, and it can still be used if it is qualified. 5406 If one of the indicators in the inspection does not meet the requirements of this standard, samples should be selected from the double amount of packaging for re-inspection. If one of the indicators in the re-inspection still does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have obvious markings, including: "food additives", product name, trademark, manufacturer name, manufacturer address, specifications, batch number, production date, production license number, and number of bottles. 6.2 Each bottle of product leaving the factory should be accompanied by a quality certificate, including: manufacturer name, product name, batch number, production date, net content, usage, shelf life, proof that the product quality meets this standard, and standard number. 6.3 Food additive temptation red aluminum lake is packed in polyethylene plastic bottles, 0.15kg per bottle, and every 10 bottles are sealed in an outer box. 6.4 It must be protected from rain, moisture, and sunlight during transportation. It should be stored in a dry and cool warehouse. 6.5 This product must not be mixed, transported or stacked with other toxic or harmful substances during storage and transportation. 6.6 The shelf life of this product is five years from the date of production. If it is overdue, it must be re-inspected to see if it meets the requirements of this standard. If it is qualified, it can still be used.6 If one of the indicators in the inspection does not meet the requirements of this standard, samples should be selected from the double amount of packaging for re-inspection. If one of the indicators in the re-inspection still does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have obvious markings, including: "food additives", product name, trademark, manufacturer name, manufacturer address, specifications, batch number, production date, production license number, and number of bottles. 6.2 Each bottle of product leaving the factory should be accompanied by a quality certificate, including: manufacturer name, product name, batch number, production date, net content, usage, shelf life, proof that the product quality meets this standard, and standard number. 6.3 Food additive temptation red aluminum lake is packed in polyethylene plastic bottles, 0.15kg per bottle, and every 10 bottles are sealed in an outer box. 6.4 It must be protected from rain, moisture, and sunlight during transportation. It should be stored in a dry and cool warehouse. 6.5 This product must not be mixed, transported or stacked with other toxic or harmful substances during storage and transportation. 6.6 The shelf life of this product is five years from the date of production. If it is overdue, it must be re-inspected to see if it meets the requirements of this standard. If it is qualified, it can still be used.
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.