Some standard content:
GB4480.2—2001
All technical contents of this standard are mandatory.
This standard is a revision of GB4480.2—1994 "Food Additives - Carmine Aluminum Lake".
The main differences between this standard and GB4480.2-1994 are as follows: Test method for heavy metals (measured in Pb): GB4480.2-1994 is atomic absorption spectrophotometry, while this standard is limited colorimetric chemical analysis.
This standard has revised the inspection rules and the terms of marking, packaging, transportation, storage, etc. From the date of implementation of this standard, it will replace GB4480.2-1994. This standard is proposed by the State Administration of 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. The drafting units of this standard: Shanghai Dye Research Institute and Shanghai Municipal Health Bureau Health Supervision Institute. The main drafters of this standard are Ding Deyi, Liu Jing, Xiao Jie, Shi Huaijiong and Zhou Yanqin. The Chemical Industry Branch of the National Technical Committee for Standardization of Food Additives is entrusted with the interpretation of this standard. This standard was first issued in 1994.
1 Scope
National Standard of the People's Republic of China
Food Additive
Carmine Aluminum Lake
Food additive--Ponceau 4R aluminum lakeGB 4480.2—2001
Replaces GB4480.2-1994
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation and storage of the food additive carmine aluminum lake. This standard is applicable to the use of colorants in food, cosmetics and other industries. Molecular formula C2HN,OS
Relative molecular mass 538.54 (according to the 1997 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. ：Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents GB/T 601—1988
GB/T 602-—1988
GB/T 603—1988
Preparation of standard solutions for determination of impurities in chemical reagents Preparation of preparations and products used in test methods of chemical reagents GB 4480.1—2001
Food additives
Carmine
Specifications and test methods for water for analytical laboratories (neqISO3696:1987)GB/T6682—1992
3 Requirements
3.1 Appearance: red powder.
3.2 Quality requirements: Should conform to the specifications in Table 1: Table 1
Content (as color acid)
Loss on drying
Insoluble matter in hydrochloric acid and ammonia water
Chloride (as NaCl) and sulfate (as Na,SO,)Subsidiary dye
(as As)
Heavy metal (as Pb)
Tonnage (as Ba)
Test method
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T6682. Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on October 24, 2001 372
2002-06-D1 implementation
GB 4480.2—2001
The standard solution, impurity standard solution, preparation and product required for the test shall be prepared in accordance with the provisions of GB/T601.GB/T602GB/T603 unless otherwise specified.
4.1 Appearance
The result shall be determined visually under natural light conditions and shall comply with the provisions of 3.1 of this standard. 4.2 Identification
4.2.1 Reagents and materials
4.2.1.1 Sulfuric acid.
4.2.1.2 Sulfuric acid solution: 1+20.
4.2.1.3 Hydrochloric acid solution: 1-3.
4.2.1.4 Ammonium acetate solution: 1.5g/L.
4.2.1.5 Sodium hydroxide solution: 100g/L. 4.2.2 Instruments and equipment
Spectrophotometer,
4.2.3 Test method
4.2.3.1 Weigh about 0.1g of the sample, add 5ml of sulfuric acid, stir and heat in a water bath from time to time, and it will turn red in about 5min. After cooling, take 2~~3 drops of the upper clear solution and add 5ml of water. It will turn red. 4.2.3.2 Weigh about 0.1g of the sample, add 5ml of sulfuric acid solution, heat and dissolve in a water bath, add ammonium acetate solution to 100mL, and then absorb 2ml. Use ammonium acetate solution to make up to 100ml. The maximum absorption wavelength of the solution should be (508±2)nm. 4.2.3.3 Weigh about 0.1g of the sample, add 10mL of hydrochloric acid solution, heat in a water bath to dissolve most of it, add 0.5g of activated carbon, shake thoroughly and filter. The solution is clear and red. Cool the solution and neutralize it with sodium hydroxide until a red 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 an alkaline medium, the azo group in the dye is reduced and decomposed into an amino compound by titanium trichloride. The percentage of the dye is calculated according to the consumption of titanium trichloride standard titration solution.
4.3.7.2 Reagents and materials
a) Trisodium citrate;
b) Standard titration solution of titanium trichloride: c(TiCl.) = 0.1 mol/L (newly prepared, see Appendix A of GB4480.12001 for preparation method):
c) Carbon dioxide in a cylinder.
4.3.1.3 Analysis steps
Weigh about 7 grams of the sample, accurate to 0.0002 μg. Add 10g of trisodium citrate, 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, shake well, draw 50mL, place in a 500ml conical flask, add 15g of trisodium citrate and 200ml of water, install the instrument according to Figure 1 in GB4480.1-2001, 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 analytical results
Express the content of carmine aluminum lake (X) in mass percentage and calculate it according to formula (1): Xt = V××0.134 6 × 100 =y×c× 67.3m×250
Wherein: V--·volume of titanium trichloride standard titration solution consumed for titrating the sample, mL; c--actual concentration of titanium trichloride standard titration solution, mol/L; m--·mass of the sample·;
GB 4480. 2-2001
0.1346---mass of carmine aluminum lake equivalent to 1.00 mL titanium trichloride standard titration solution [c(TiCl)=1 mol/L], expressed in grams.
4.3.1.5 Allowable difference
The difference between two determination results of the same sample 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 Method summary
After the sample and the standard sample with known content are dissolved in water respectively, their absorbance is measured at the maximum absorption wavelength respectively, and then the content of the sample is calculated.
4.3.2.2 Reagents and materials
a) Trisodium citrate;
b) Carmine standard sample: ≥85.0%; the content is determined by titanium trichloride titration method. 4.3.2.3 Instruments and equipment;
a) Spectrophotometer;
b) Colorimetric III: 10mm.
4.3.2.4 Preparation of Carmine Standard Solution
Weigh 0.5g of Carmine Standard Solution, accurate to 0.0002g. Dissolve in an appropriate amount of water, transfer to a 1000mL volumetric flask, dilute to the mark, and shake well. Pipet 10mL, transfer to a 500mL volumetric flask, dilute to the mark, and shake well. 4.3.2.5 Preparation of Carmine Aluminum Lake Sample Weigh about 2.125g of Carmine Aluminum Lake Sample, accurate to 0.0002g. Add 20mL of water and about 2g of trisodium citrate, slowly heat to 90℃, and the rest is the same as the preparation of Carmine Standard Solution. 4.3.2.6 Analysis Steps
Measure the absorbance of the standard solution and the sample solution at a wavelength of (508±2)nm on a spectrophotometer using a 10mm colorimetric filter.
Water is used as the reference liquid.
4.3.2.7 Expression of analysis results
The content of aluminum lake of carmine expressed as mass percentage (X,) is calculated according to formula (2): mAX.
× 100
Wherein: A-
Absorbance of test solution;
A--Absorbance of standard solution;
X. —Mass percentage of carmine standard sample (titanium trichloride method); ml---Mass of standard sample;
m-Mass 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 loss on drying
Perform according to 4.4 of GB4480.1-2001.
4.5 Determination of insoluble matter in hydrochloric acid and ammonia water 4.5.1 Reagents and materials
4.5.1.1 Hydrochloric acid.
4.5.1.2 Hydrochloric acid solution: 3+7.
4.5.1.3 Ammonia solution: 4+96.
4. 5. 1.4
Silver nitrate solution: c(AgNO.)=0.1mol/L. (2)
4.5.2 Analysis steps
GB 4480. 2--2001
Weigh about 2g of sample, accurate to 0.01g. In a 600mL beaker, add 20mL of water and 20mL of hydrochloric acid. Stir thoroughly and 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 that has been dried to constant weight at (135±2)℃. Rinse the insoluble matter in the beaker into a crucible with water until the washing solution is colorless, then wash with 10mL of ammonia solution, wash with 10mL of hydrochloric acid solution, and then wash with water until the solution is free of white precipitation when tested with silver nitrate solution, then place in a (135±2)℃ constant temperature oven and dry to constant weight.
4.5.3 Expression of analysis results
Express the insoluble matter content in hydrochloric acid and ammonia water (X,) in mass percentage, calculated according to formula (3): m2×100
--mass of insoluble matter after drying, 8;
Where: mz--
m--mass of sample·g.
4.5.4 Allowable difference
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. 4.6 The determination of chloride (calculated as NaCl) and sulfate (calculated as Na.SO,) content shall be carried out in accordance with 4.5 of GB4480.1-2001.
The total mass percentage of chloride (calculated as NaCl) and sulfate (calculated as Na2SO,) shall not exceed 2.0%. 4.7 Determination of secondary dye content
4.7.1 Reagents and materials
4.7.1.1 Anhydrous ethanol.
4.7.1.2 Butanol.
4.7.1.3 Acetone solution: 1+1.
4.7.1.4 Ammonia solution: 4+96.
Sodium bicarbonate solution: 4g/L.
4.7.1.6 Trisodium citrate.
4.7.2 Instruments and equipment
4.7.2.1 Spectrophotometer.
4.7.2.2 Chromatographic filter paper: No. 1 medium speed, 150mm×250mm, 4.7.2.3 Chromatographic cylinder: 240mm×300mm. 4.7.2.4 Micro-injector: 100uL.
4.7.3 Analysis steps
4.7.3.1 Paper chromatography conditions
a) Developing solvent: n-butanol + anhydrous ethanol + ammonia solution = 6+2+3. h) Temperature: 20~25C.
(3)
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 5g of trisodium citrate, slowly heat to 400C, stir to dissolve, transfer to a 100ml volumetric flask, dilute to scale, and shake well. Use a microinjector to accurately draw 200uL, 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 a chromatography cylinder that has been saturated with solvent in advance to develop, and immerse the bottom edge of the filter paper 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 it dry with a hair dryer with cold air. At the same time, use a blank filter paper to develop under the same conditions. The blank filter paper must be cut from the adjacent part of the filter paper (60) mm × 600 mm) used for developing the sample solution. 375
GB 4480.2—2001
Schematic diagram of chromatography on paper of secondary dyes
Secondary dyes (1)
Secondary dyes (2)
Main dye
Secondary dyes (3)
Secondary dyes (4)
Cut each secondary dye and the filter paper corresponding to each secondary dye on the blank filter paper into the same size and cut into 5mm×15mm thin strips. Place them in 50ml Nessler colorimetric tubes respectively. Accurately add 5ml of acetone solution to each tube. Shake for 3~～5min, then accurately add 20ml of sodium bicarbonate solution and shake thoroughly. Filter the extracts naturally in No. 3 glass frit funnels. The filtrate must be clear and free of suspended matter. Use a 50mm colorimetric III at the maximum absorption wavelength of each secondary dye and a spectrophotometer to measure the absorbance at the maximum absorption wavelength of each secondary dye.
Use a mixture of 5ml of acetone solution and 20ml of sodium bicarbonate solution as the reference solution. 4.7.3.3 Preparation of standard eluate
Pipette 6ml of the above 2% sample solution, transfer it into a 100ml volumetric flask, dilute to the mark, and shake well. Use a micro-injector to draw 200μL, evenly apply it on a baseline 25mm away from the bottom edge of the filter paper, blow it dry with cold air, put the filter paper into a chromatography cylinder that has been saturated with solvent in advance and develop it. When the front line of the developing agent rises only 40mm, take it out and blow it on all the cut dye parts. The extraction operation is the same as before, and the absorbance is measured at the maximum absorption wavelength using a 10mm colorimetric III. At the same time, use a blank filter paper to develop it under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.4 Expression of analysis resultswww.bzxz.net
Express the content of carmine aluminum lake secondary dye (X.) in mass percentage. Calculate according to formula (4): X. - [(A-6) ++(4. - b)]/5 × 6 × sAb
Wherein. A,.,A.
Absorbance of each secondary dye extract calculated at 50 mm optical path length; absorbance of each secondary dye reference blank extract calculated at 50 mm optical path length; h,.,h.
Absorbance of standard extract calculated at 10 mm optical path length; A.
b, absorbance of standard reference blank sample calculated at 10 mm optical path length; 5-ratio converted to 10 mm optical path length: 6-
reference concentration of standard extract based on 2% sample solution, %, S total content of sample.
4.7.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.8 Determination of arsenic content
(4)
According to 4.8 of GB4480.1-2001.
4.9 Determination of heavy metal content
4.9.1 Reagents and materials
4.9.1.1 Hydrochloric acid.
4.9.1.2 Nitric acid.
4.9.1.3 Ammonia water.
4.9.1.4 Sulfuric acid solution: 1+1.
4.9.1.5 Hydrochloric acid solution: 1+3.
4.9.1.6 Ammonium acetate solution: 1+9.
4.9.1.7 Nitric acid-perchloric acid mixture: 3+1. 4.9.1.8 Sodium sulfide solution: 100g/L.
GB4480.2—2001
4.9.1.9 Lead standard solution (0.01mg/mL): Take 10mL of 0.1mg/mL lead standard solution in a 100mL volumetric flask and dilute to the scale.
4.9.2 Analysis steps
Weigh 2.5g of the sample to an accuracy of 0.01g. Place in a round-bottom flask, add 5-8mL nitric acid to wet the sample, place for a while, heat slowly, wait for the effect to ease and cool slightly, add 10-12mL sulfuric acid solution along the wall of the flask, and heat slowly until the solution in the flask begins to turn brown, stop heating, cool and add 5mL of nitric acid-perchloric acid mixture, continue heating until a large amount of sulfur dioxide white smoke is generated, and the solution should be colorless or slightly yellow (if it is still yellow, add more mixture to treat). After cooling, add 20mL of water, boil to remove the residual nitric acid until white smoke is generated, do this twice, and cool. Transfer the solution to a 50mL volumetric flask, wash the round-bottom flask with water, add the washing liquid to the volumetric flask, add water to the scale, mix well, and use it as the sample solution. Take the same amount of nitric acid and sulfuric acid solution and use the above method as the blank test solution. Measure 20mL of the sample solution, adjust the pH with ammonia water, and then add ammonium acetate solution to adjust the pH to about 4. Add water to 50mL as the test solution. Separately, measure 20ml of blank test solution and 2.0ml of lead standard push solution, and perform the same operation as the sample to prepare a comparative solution. Add 2 drops of sodium sulfide test solution to each solution, shake well, and let stand for 5 minutes. The color of the test solution should not be darker than that of the comparative solution. 4.10 Determination of lock content
4.10.1 Reagents and materials
4.10.1.1 Sulfuric acid.
4.10.1.2 Sulfuric acid solution: 1+19.
4.10.1.3 Hydrochloric acid solution: 1+3.
4.10.2 Analysis steps
Accurately weigh 1g of the sample to the nearest 0.01g. Place in a platinum (porcelain or quartz) 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, slowly heat until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450~550C for 3h. After cooling, 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, dissolve the molten material, cool, 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 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, then add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution, mix, and leave for 10 minutes, it should not be turbid.
5 Inspection rules
5.1 Items specified in this standard: Except for the determination of barium content, which is a type inspection, under normal production conditions, type inspection is carried out at least once a quarter, all other items are factory inspection items, including content (in color acid), drying loss, insoluble matter in hydrochloric acid and ammonia water, chloride (in NaCl) and sulfate (in NaSO,), secondary dyes, arsenic (in As), and heavy metals (in Pb) test items should be inspected batch by batch. 377
GB4480.2-2001
5.2 Food additive carmine aluminum lake, the quality inspection department of the production unit shall inspect the product quality according to the provisions of this standard. The production unit shall ensure that the quality of all food additive carmine aluminum lakes shipped out of the factory meets the requirements of this standard and has a quality certificate in a certain format.
5.3 Food additive carmine aluminum lakes, a batch is a uniform product mixed at one time. 5.4 Bottled product sampling should be selected from the total number of packaging boxes (each box is 10×150g) of each batch of products, 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. After the sample is quickly mixed, take about 100g from it and put it in two clean and dry containers, respectively, and seal them, and label them with the manufacturer name, product name, batch number, and sampling date. One copy is for inspection and the other is kept for reference. The manufacturer can sample and inspect the products that are mixed uniformly before packaging, and the sampling volume shall not be less than 200g. 5.5 If one of the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. If one of the test results still does not meet the requirements of this standard, the batch of products shall be deemed unqualified. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have firm and clear markings, including: "Food additives, product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, shelf life. 6.2 Each bottle of product leaving the factory should have obvious markings, including: "Food additives, product name, manufacturer name and address, trademark, production and food hygiene license number, product promotion number and standard name, shelf life, production date and batch number, net content, instructions for use. 6.3. The food additive carmine aluminum lake is packed in food-grade polyethylene plastic bottles, 150g per bottle + sealed outer box for every 10 bottles. Other forms of packaging can be determined by negotiation between the manufacturer and the user. 6.4 During transportation, the product must be protected from rain, moisture and sunlight, and should be stored in a dry, cool warehouse. 6.5 During storage and transportation, the product must not be mixed, transported or stacked with other toxic or harmful substances. 6.6 The shelf life of this product is five years from the date of production. If it is overdue, it can be re-inspected to see if it meets the requirements of this standard. If it is qualified, it can still be used.5 If one of the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. If one of the test results still does not meet the requirements of this standard, the batch of products shall be deemed unqualified. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have firm and clear markings, including: "Food additives, product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, shelf life. 6.2 Each bottle of product leaving the factory should have obvious markings, including: "Food additives, product name, manufacturer name and address, trademark, production and food hygiene license number, product promotion number and standard name, shelf life, production date and batch number, net content, instructions for use. 6.3. The food additive carmine aluminum lake is packed in food-grade polyethylene plastic bottles, 150g per bottle + sealed outer box for every 10 bottles. Other forms of packaging can be negotiated and determined by the manufacturer and the user. 6.4 During transportation, the product must be protected from rain, moisture and sunlight, and should be stored in a dry, cool warehouse. 6.5 During storage and transportation, the product must not be mixed, transported or stacked with other toxic or harmful substances. 6.6 The shelf life of this product is five years from the date of production. If it is overdue, it can be re-inspected to see if it meets the requirements of this standard. If it is qualified, it can still be used.5 If one of the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. If one of the test results still does not meet the requirements of this standard, the batch of products shall be deemed unqualified. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have firm and clear markings, including: "Food additives, product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, shelf life. 6.2 Each bottle of product leaving the factory should have obvious markings, including: "Food additives, product name, manufacturer name and address, trademark, production and food hygiene license number, product promotion number and standard name, shelf life, production date and batch number, net content, instructions for use. 6.3. The food additive carmine aluminum lake is packed in food-grade polyethylene plastic bottles, 150g per bottle + sealed outer box for every 10 bottles. Other forms of packaging can be negotiated and determined by the manufacturer and the user. 6.4 During transportation, the product must be protected from rain, moisture and sunlight, and should be stored in a dry, cool warehouse. 6.5 During storage and transportation, the product must not be mixed, transported or stacked with other toxic or harmful substances. 6.6 The shelf life of this product is five years from the date of production. If it is overdue, it can be re-inspected to see if it meets the requirements of this standard. If it is qualified, it can still be used.
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