Some standard content:
GB 6227.1—1999
This standard adopts the 6th edition of the Japanese Food Additives Standard (1992) in a non-equivalent manner. GB6227.1-1995 has been revised based on the standard for "Edible Yellow No. 5 (Sunset Yellow)" in the book. The main technical differences between this standard and the Japanese standard are as follows: 1. The content index of this standard is ≥85.0% and the content index of ≥60.0% is reserved, while the content index of Japan is ≥85.0%. 2. The total amount of drying loss, chloride (calculated as NaCl) and sulfate (calculated as Na, SO.) in Sunset Yellow 85 of this standard is ≤15.0%, while the Japanese standard recommends that the drying loss index is ≤10.0%, and the chloride and sulfate indexes are ≤5.0%. 3. The content index of heavy metals (calculated as Pb) in this standard is ≤0.001%, while the index of Japan is ≤0.002%. 4. The content determination of secondary dyes in this standard continues to follow GB6227.1-1995, adopts the determination method in FAO/WHO, and the index is ≤4.0%.
5. The content determination of steatite in this standard adopts the determination method of steatite in food additives in GB/T8450-1987, and the index is ≤0.0001% (as As), and the Japanese index is ≤0.0004% (As2O.). 6. In addition to the titanium trichloride titration method, the content determination in this standard adds a relatively simple spectrophotometric method for daily determination. The titanium trichloride method is used as the arbitration method.
7. The determination method of chloride (as NaCl) and sulfate (as Na2SO.) in this standard is chemical titration, and the Japanese standard adopts ion chromatography.
The main differences between this standard and GB6227.1-1995 are as follows: 1. GB6227.1-1995 has two specifications, Sunset Yellow 85 and Sunset Yellow 60. Sunset Yellow 60 in this standard is the reserved specification. 2. In the Sunset Yellow 85 specification of this standard, the drying loss, chloride (calculated as NaCl) and sulfate (calculated as Na2SO.) are combined into a total amount, and the index is ≤15.0%.
3. The content of isopropyl ether extract is cancelled. The rest is the same as GB6227.1-1995.
This standard was first issued in 1986 and revised for the second time in 1999. From the date of implementation, this standard will replace GB6227.1-1995. Appendix A in this standard is the appendix of the standard.
This standard is proposed by the State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Technical Committee on Dye Standardization and the Food Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai Dyestuff Research Institute and Shanghai Municipal Health Bureau Health Supervision Institute. The main drafters of this standard are Ding Deyi, Liu Jing, Shi Huaijiong, Cheng Chunhong, Guan Jianxiong and Zhou Yanqin. The National Technical Committee on Dyestuff Standardization is entrusted with the interpretation of this standard. 416
1 Scope
National Standard of the People's Republic of China
Food additives
Sunset yellow
Food additive-
Sunset yellow
GB6227.1—1999
Replaces GB6227.111995
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation and storage of food additive sunset yellow. This standard applies to dyes obtained by coupling p-aminobenzenesulfonic acid with sodium 2-phenol-6-sulfonate after diazotization. Structural formula:
Molecular formula: CH.N,O,S2Na2
Relative molecular mass: 452.37 (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/T601—1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents Preparation of standard solutions for determination of impurities in chemical reagents GB/T 602—1988
GB/T603—1988 Preparation of preparations and products used in test methods for chemical reagents GB/T6682—1992 Specifications and test methods for water used in analytical laboratories GB/T 8450—1987
3 Requirements
Determination of impurities in food additives
3.1 Appearance Orange-red powder.
3.2 The quality of food additive Sunset Yellow 85 shall meet the requirements of Table 1. Approved by the State Administration of Quality and Technical Supervision on July 12, 1999, and implemented on January 1, 2000
GB6227.1 - 1999
Requirements in Table 1
Loss on drying, chloride (as NaCl) and sulfate (as NazSO,) Total water-insoluble matter
Subsidiary dye
Arsenic (as As)
Heavy metal (as Pb)
The quality of food additive Sunset Yellow 60 shall meet the requirements of Table 2. Sunset Yellow 60 is a reserved specification. 3.3
Requirements in Table 2
Loss on drying
Permanently insoluble matter
Subsidiary dye
Arsenic (as As)
Heavy metal (as Pb)
Note: Reserved specifications are those that are restricted in development and are to be cancelled. 4
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. 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 unless otherwise specified.
4.1 Appearance
Visual determination
4.2 Identification
4.2.1 Reagents and materials
a) Sulfuric acid solution: 1+100;
b) Ammonium acetate solution: 1.5g/L,
4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Test method
4.2.3.1 Weigh about 0.1g of sample and dissolve it in 100mL of water to form an orange clear solution. 4.2.3.2 Take 40mL of the orange solution in 4.2.3.1 and add 10mL of sulfuric acid solution to form an orange-red solution. Take 2-3 drops of this solution and add it to 5mL of water to form an orange-yellow solution.
4.2.3.3 Weigh 0.1g of sample and dissolve it in 100mL of ammonium acetate solution. Take 1mL of this solution and add ammonium acetate solution to make it 100mL. The maximum absorption wavelength of this solution is 482nm±2nm. 4.3 Determination of content
4.3.7 Titanium trichloride titration method (arbitration method)4.3.1.1 Summary of the method
GB 6227. 1 1999
In an alkaline medium, the azo group in the sample is reduced and decomposed by titanium trichloride. The percentage content of the dye is calculated according to the consumption of titanium trichloride standard titration solution.
4.3.1.2 Reagents and materials
a) Sodium hydrogen tartrate;
b) Titanium trichloride standard titration solution c(TiCl) = 0.1 mol/L (freshly prepared, see Appendix A for preparation method); c) Carbon dioxide in a cylinder.
4.3.1.3 Test method
Weigh 5 g of Sunset Yellow 85 or Sunset Yellow 60 sample, accurate to 0.0002 g, dissolve in 100 mL of freshly boiled water cooled to room temperature, transfer to a 500 mL volumetric flask, dilute to the mark, shake well, accurately pipette 50 mL, place in a 500 mL conical flask, add 15 g of trisodium citrate and 150 mL of water, assemble the instrument as shown in Figure 1, heat to boiling while passing a stream of carbon dioxide gas under the liquid surface, and titrate with titanium trichloride standard titration solution until the colorless end point is reached.
Erlenmeyer flask (500ml); 2-brown burette (50mL); 3-glass bottle with a black paper wrapper (2000mL); 4-container for a mixture of 10% ammonium carbonate and 10% ferrous sulfate (5000mL); 5-piston: 6-empty bottle; 7-wash bottle filled with water
Figure 1 Apparatus diagram of titanium trichloride titration method
4.3.1.4 Expression of analysis results
Express the content of sunset yellow (X,) in mass percentage and calculate according to formula (1): Xx -XcX0.1131 × 100
V Xcx 113. 1
Where: V-the volume of titanium trichloride standard titration solution consumed for titration of the sample, ml; c--the actual concentration of titanium trichloride standard titration solution, mol/L; 12
m--the mass of the sample, g;
0.1131~-the mass of sunset yellow in grams equivalent to 1.00m titanium trichloride standard titration solution L(TiCl,)=1.000mol/L1, 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 colorimetry
4.3.2.1 Method summary
GB 6227. 1-- 1999
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
Sunset Yellow 85 or Sunset Yellow 60 standard sample: homemade, the content is determined by titanium trifluoride titration method. 4.3.2.3 Instruments and equipment
a) Spectrophotometer;
b) Colorimetric dish: 10mm.
4.3.2.4 Preparation of Sunset Yellow 85 or Sunset Yellow 60 Standard Solution Weigh 0.5g of Sunset Yellow 85 or Sunset Yellow 60 standard sample, accurate to 0.0002g, dissolve in an appropriate amount of water, transfer to a 1000mL volumetric flask, dilute to the mark, and shake well. Accurately pipette 10mL, transfer to a 500mL volumetric flask, dilute to the mark, and shake well. 4.3.2.5 Preparation of Sunset Yellow 85 or Sunset Yellow 60 Test Solution Weigh 0.5g of the sample, and the rest is the same as the preparation of the standard solution. 4.3.2.6 Test Method
Place the standard solution and the test solution in a 10mm colorimetric solution, and measure their respective absorbances at a wavelength of 482nm±2nm using a spectrophotometer.
Use water as reference solution
4.3.2.7 Expression of analysis results
Express the content of Sunset Yellow 85 or Sunset Yellow 60 in mass percentage (X) according to formula (2): X
Wherein: A—absorbance of sample solution; A.—absorbance of standard solution;
X—mass percentage of Sunset Yellow 85 or Sunset Yellow 60 standard sample (titanium trichloride method). 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, total amount of chloride (calculated as NaCl) and sulfate (calculated as Na2SO,). 4.4.1 Determination of loss on drying
4.4.1.1 Test method
Weigh about 2g of sample, accurate to 0.01g, place in a (30~40)mm weighing bottle that has been weighed to a constant weight, and dry in a constant temperature oven at 135℃±2C to constant weight.
4.4.1.2 Expression of analysis results
Express the content of loss on drying as mass percentage (X.) Calculate according to formula (3): X
Where: m2——mass of sample before drying·g, m
mass of sample after drying to constant weight, g.
m×100
4.4.7.3 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. 4.4.2 Determination of chloride (as NaCl) content 4.4.2.1 Reagents and materials
a) Activated carbon;
b) Nitrobenzene;
c) Nitric acid solution: 1+1;
GB6227, 1-1999
d) Silver nitrate standard titration solution: c(AgNO:)=0.1mol/L; e) Ammonium thiocyanate standard titration solution: c(NH,CNS)=0.1mol/I; f) Ammonium ferric sulfate solution;
Preparation: Weigh 14g of ammonium ferric sulfate, dissolve it in 100mL of water, filter, add 10mL of nitric acid, and store in a brown bottle. 4.4.2.2 Preparation of test solution
Weigh about 2g of Sunset Yellow 85 sample, accurate to 0.01g + add 200mL of water, add 10g of activated carbon, and then add 1mL of nitric acid solution, stir evenly, place for 30min (stir from time to time), filter with dry filter paper, if the filtrate is colored, add 2g of activated carbon, stir from time to time and place for 1h, then filter with dry filter paper, if it is still colored, replace the activated carbon and repeat the operation. 4.4.2.3 Test method
Pipette 50mL of the above test solution, place it in a 500mL conical flask, add 2mL of nitric acid solution and 10ml of silver nitrate standard titration solution. (Add more when the chloride content is high) and 5mL of nitrobenzene, shake vigorously until the silver chloride condenses, add 1ml of ammonium ferric sulfate solution, and titrate with ammonium thiocyanate standard titration solution until the solution turns brick red as the end point and keep for 1min. At the same time, do a blank test in the same way. 4.4.2.4 Expression of analytical results
Express the chloride content (in terms of NaCl) in mass percentage (X) and calculate it according to formula (4): X, = -V) × 0.0584 × 100 = (V-V) × c × 23.36m × 200
Wherein: V is the volume of ammonium thiocyanate standard titration solution consumed in titrating the sample, mL; V is the volume of ammonium thiocyanate standard titration solution consumed in titrating the blank solution, mL; m is the actual concentration of the ammonium thiocyanate standard titration solution, mol/I;
m is the mass of the sample, g;
0.0584 is the mass of sodium chloride in grams equivalent to 1.00mL of ammonium thiocyanate standard titration solution [c(NH,CNS)1.000mal/L].
4.4.2.5 Allowable difference
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. 4.4.3 Determination of sulfate (in terms of NVa2SO.) content 4.4.3.1 Reagents and materials
a) Ammonia water;
b) Sodium hydroxide solution: 0.2g/L;
c) Hydrochloric acid solution: 1+99:
d) Ethanol: 95%:
e) Disodium tetrahydroxybenzoaldehyde-potassium chloride: Mix the indicator in equal amounts; f) Standard sulfuric acid titration solution: c(1/2H, SO4）=0.1mol/L;g）phenolic acid indicator solution: 10g/L;
h）sodium rose bengalate indicator solution: weigh 0.1g sodium rose bengalate, dissolve in 10mL water (prepare and use immediately);i) barium chloride standard titration solution: c(1/2BaCl2)=0.1mol/L; 1. Preparation: weigh 12.25g barium chloride, dissolve in 500mL water, transfer to a 1000mL volumetric flask, dilute to scale, shake and hook. 1. Calibration: absorb 20mL sulfuric acid standard solution, add 50mL water, and neutralize with ammonia water until the bright yellow test paper shows alkaline reaction, then titrate with barium chloride standard solution, use sodium rose bengalate indicator solution as extra-liquid indicator, and the end point is when a rose red spot appears on the filter paper and remains for 2 minutes without fading.
The concentration of barium chloride standard titration solution (X:) is calculated according to formula (5): XgKxc
. (5)
Wherein: V-
GB 6227. 1—1999
Volume of standard sulfuric acid titration solution, mL:
Volume of standard barium chloride titration solution, mL; actual concentration of standard sulfuric acid titration solution, mol/L. 4.4.3.2 Test method
Pull 25mL of the test solution into a 250mL conical flask, add 1 drop of phenolic acid indicator solution, add sodium hydroxide solution until it turns pink, then add hydrochloric acid solution until the pink color disappears, then add 30mL of ethanol and 0.4g of tetrahydroxybenzoaldehyde disodium-potassium chloride mixed indicator, shake the hook, and after dissolution, titrate with barium nitride standard solution under continuous shaking until the solution turns rose red as the end point. During the titration, illuminate with light from the side and observe carefully. Use rose red sodium acid indicator solution as an extra-liquid indication for comparison. At the same time, perform a blank test in the same way. 4.4.3.3 Expression of analytical results
Express the sulfate content (in terms of Na2SO4) in mass percentage (X.) and calculate it according to formula (6): (V - V) X c X 0.071 x
(V - V) X c X 56.8
Wherein: V -
. (6)
The volume of barium chloride standard titration solution consumed in titrating the sample solution, mL; The volume of barium chloride standard titration solution consumed in titrating the blank solution, mL; The actual concentration of barium chloride standard titration solution, mol/L The mass of the sample, g:
The mass of 0.071-
of sodium sulfate equivalent to 1.00mL of barium chloride standard titration solution [c(1/2BaCl.)=1.000mol/L], expressed in grams, g.
4.4.3.4 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. ·4.4.4 Expression of analysis results
The sum of the content of drying loss, the content of chloride (in terms of NaCl) and the content of sulfate (in terms of Na2SO4) expressed in mass percentage (X,) shall be calculated according to formula (7):
X,= X +X +X.
Where: X,-
Express the drying loss content in mass percentage, %; X. ——Express the chloride content in mass percentage, %; X, —Express the sulfate content in mass percentage, %. 4.5 Determination of water-insoluble content
4.5.1 Determination method
Weigh about 3g of sample, accurate to 0.01g, place in a 500mL beaker, add 250mL of 50℃～60℃ water to dissolve it, filter with a No. 4 glass sand core that has been dried to constant weight at 135E±2℃, and wash thoroughly with hot water until the washing liquid is colorless, and dry in a constant temperature oven at 135C±2℃ to constant weight.
4.5.2 Expression of analysis results
Express the water-insoluble content (X.) in mass percentage. Calculate according to formula (8): m2×100
Where: m3--the mass of water-insoluble matter after drying·g the mass of the sample, g.
4.5.3 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 Determination of secondary dye content
4.6.1 Method summary
GB 6227. 1-1999
Separate and elute the components by paper chromatography, and then quantify by spectrophotometry. 4.6.2 Reagents and materials
a) Anhydrous ethanol
b) n-butanol;
r) Acetone solution: 1+1;
d) Ammonia solution: 4+96;
e) Sodium bicarbonate solution: 4g/L.
4.6.3 Instruments and equipment
a) Spectrophotometer:
b) Chromatographic filter paper: No. 1 medium speed, 150mm×250mm; c) Chromatographic cylinder: $240mmX300mm;
d) Micro-injector: 100μL.
4.6.4 Test method
4.6.4.7 Paper chromatography conditions
a) Developing solvent: n-butanol + anhydrous ethanol + ammonia solution = 6+2+3;
b) Temperature: 20C~25C.
4.6.4.2 Preparation of sample eluate
Weigh 1g of Sunset Yellow 85 or Sunset Yellow 60 sample, accurate to 0.01g, place in a beaker, add appropriate amount of water to dissolve, transfer to a 100ml volumetric flask, dilute to scale, shake, and use a microinjector to draw 200μL, evenly apply it on a baseline 25mm away from the bottom edge of the filter paper to form a straight line, so that the width of the solution on the filter paper does not exceed 5mm and the length is 130mm. Blow it dry with a hair dryer, put the filter paper in the chromatography tank for development, and immerse the bottom edge of the filter paper 10mm below the liquid surface of the developer. When the front line of the developer rises to 150mm or until the secondary dye is separated satisfactorily, take out the chromatography filter paper, blow it dry with cold air from a hair dryer, and develop it with a blank filter paper under the same conditions (the blank filter paper must be cut from the adjacent part of the filter paper used for developing the test solution on the same 600mmX600mm filter paper). 150mm
-Subsidiary dye (1)
Subsidiary dye (2)
Main dye
A secondary dye (3)
Subsidiary dye (4)
Figure 2 Schematic diagram of secondary dye chromatography
GB 6227. 1-1999
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 thin strips of about 5mmX15mm. Place them in 50mL Nessler colorimetric tubes respectively, add 5mL of acetone solution to each tube, shake for 3min~5min, and then accurately add 20ml of sodium bicarbonate solution. Shake thoroughly, and filter the extracts naturally in No. 3 glass sand core funnels respectively. The filtrate must be clear and free of suspended matter. Use 50mm colorimetric III to measure the absorbance on a spectrophotometer at the maximum absorption wavelength of each secondary dye. Use a mixture of 5 mL of acetone solution and 20 mL of sodium bicarbonate solution as the reference solution. 4.6.4.3 Preparation of standard eluate
Accurately pipette 2 mL of the above 1% sample solution into a 100 mL volumetric flask, dilute to the mark, and shake. Use a micro-injector to pipette 200 μl, evenly apply it on a baseline 25 mm from the bottom edge of the filter paper, blow dry with cold air, put the filter paper into the chromatography cylinder for development, wait until the front line of the developing agent rises only 40 mm, take it out and blow dry, cut off all the dye parts, perform the extraction operation as before, and measure the absorbance at the maximum absorption wavelength with a 10 mm thick colorimetric III
At the same time, use a blank filter paper for development under the same conditions, and measure the absorbance of the extract after the same operation. 4.6.4.4 Expression of analysis results
Express the content of accessory dye (X.) in mass percentage and calculate it according to formula (9): (At - b)-:
..... -- (A. - bn)
Wherein: A.*,A.-
Absorbance of each accessory dye extract calculated at a light path length of 50 mm; Absorbance of each accessory dye reference blank extract calculated at a light path length of 50 mm; Absorbance of standard extract calculated at a light path length of 10 mm; 6.-Absorbance of standard reference blank extract calculated at a light path length of 10 mm; 5---Ratio converted to calculation based on a light path length of 10 mm; 2-
-Reference concentration of standard extract based on 1% sample solution, %; S
4.6.4.5 Allowable difference
-Total content of the sample.
The difference between the results of the two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 4.7 Determination of arsenic content
4.7.1 Reagents and materials
a) Nitric acid
b) Sulfuric acid solution: 1+1;
(9)
c) Nitric acid-perchloric acid mixture: 3+1;
d) Arsenic standard solution: 0.001mg/mL. Take 1mL of the standard solution containing 0.1mg/mL arsenic (As) in a 100mL volumetric flask and dilute to the scale.
4.7.2 Instruments and equipment
Apparatus according to the medium spot method of GB/T8450-1987. 4.7.3 Test method
Weigh 1.0g of Sunset Yellow 85 or Sunset Yellow 60 sample, accurate to 0.01g, and place it in a round-bottom flask. Add 1.5mL of nitric acid and 5mL of sulfuric acid solution. Heat with low heat to drive out nitrogen dioxide gas. When the solution turns brown, stop heating. After cooling, add 5mL of nitric acid-perchloric acid mixture. Heat with high heat until the solution is transparent, colorless or slightly yellow. If it is still opaque, add 5mL of nitric acid-perchloric acid mixture after cooling. Continue heating until the solution is clear, colorless or slightly yellow and produces white smoke. Stop heating, cool, add 5mL of water and heat to boiling to remove residual nitric acid-perchloric acid (add water and boil once if necessary). Continue heating until white smoke is produced. Keep for 10min. After cooling, transfer to a 100mL conical flask. The following shall be carried out in accordance with the provisions of 2 and 4 of GB/T8450-1987. 4.8 Determination of heavy metal content
4.8.1 Reagents and materials
a) Sulfuric acid;
b) Hydrochloric acid;
c) Hydrochloric acid solution: 1+3;
d) Acetic acid solution: 1+3
e) Ammonia solution: 1+2;
1) Sodium sulfide solution: 100g/L,
GB 6227. 1 -- 1999
g) Lead standard solution: 0.01mg/mL. Take 10mL of the standard solution containing 0.1mg/mL of lead (Pb) in a 100mL volumetric flask and dilute to the scale
4.8.2 Preparation of sample solution
Weigh 2.5g of Sunset Yellow 85 or Sunset Yellow 60 sample, accurate to 0.01g, place it in a platinum (or quartz, porcelain) flask, add a small amount of sulfuric acid to moisten it, slowly burn it, and try to make it almost completely ash at a low temperature, then add 1mL of sulfuric acid, gradually heat it until sulfuric acid vapor almost stops. Put it in an electric furnace, burn it at 450℃~550℃ until it is ash, and then cool it. Add 3mL of hydrochloric acid to shake, then add 7mL of water to shake, and filter it with quantitative analysis filter paper (No. 5C). Wash the residue on the filter paper with 5mL of hydrochloric acid solution and 5mL of water, combine the washing and filtrate, and add water to 50mL as the sample solution. Use the same method without adding sample to prepare a blank test solution. 4.8.3 Preparation of test solution
Measure 20mL of the sample solution, put it into a Nessler colorimetric tube, add 1 drop of phenolic acid test solution, add ammonia solution until the solution turns red, then add 2ml of acetic acid solution, filter if necessary, wash the filter paper with water, add water to make up to 50mL, as the test solution. 4.8.4 Preparation of comparison solution
Measure 20ml of blank test solution, put it into a Nessler colorimetric tube, add 2.0mL of lead standard solution and 1 drop of phenol indicator solution, prepare it in the same way as the test solution, as the comparison solution. 4.8.5 Test method
Add 2 drops of sodium sulfide solution to the test solution and the comparison solution respectively, shake well, and after standing for 5 minutes, the color of the test solution shall not be darker than that of the comparison solution.
5 Inspection rules
5.1 The quality inspection department of the production unit shall inspect the product quality of the food additive Sunset Yellow 85 or Sunset Yellow 60 in accordance with the provisions of this standard. The production unit shall ensure that the quality of all food additives Sunset Yellow 85 or Sunset Yellow 60 shipped from the factory meets the requirements of this standard and has a quality certificate in a fixed format.
5.2 The food additive Sunset Yellow 85 or Sunset Yellow 60 is a batch of uniformly mixed products. 5.3 For bottled products, 10% of the total number of product packaging boxes (each box is 10×0.5kg) should be selected for sampling. Then 10% of the bottles should be selected 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 sampling to prevent foreign impurities from falling into the product. Mix the collected samples quickly and take out about 100g from them. Put them in two clean, dry ground 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 Sunset Yellow 85 or Sunset Yellow 60 received in accordance with the inspection rules and test methods specified in this standard.
6 Marking, packaging, transportation, 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 obvious markings, 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 Food additive Sunset Yellow 85 or Sunset Yellow 60 is packed in polyethylene plastic bottles, 0.5kg 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. 6.5 This product shall not be mixed, transported or stacked with other toxic or harmful substances during transportation. 6.6 The shelf life of this product is five years from the date of production. It can only be used if it fully complies with the requirements of this standard after re-inspection. 126
A1 Reagents and materials
a) Hydrochloric acid:
b) Ammonium ferrous sulfate;
c) Ammonium thiocyanate solution: 200g/I;
d) Sulfuric acid solution: 1+1;
GB 6227.1—1999
Appendix A
(Appendix to the standard)
Preparation method of titanium trichloride standard titration solutione) Potassium dichromate standard titration solution: c (1/6K.Cr.0,) = 0.1mol/L. A2 Instruments and equipmentwwW.bzxz.Net
See Figure 1.
A3 Preparation of titanium trichloride standard titration solution A3.1 Preparation
Put 100 mL of titanium trichloride solution and 75 mL of hydrochloric acid in a 1000 mL brown volumetric flask, dilute to the mark with freshly boiled water that has been cooled to room temperature, shake the hook, and immediately pour into a light-proof lower-mouth bottle and store under the protection of carbon dioxide gas. A3.2 Calibration
Weigh 3g of ammonium ferrous sulfate, accurate to 0.0002g, and place it in a 500mL conical flask. Under the protection of carbon dioxide gas flow, add 50mL of freshly boiled and cooled water to dissolve it, then add 25mL of sulfuric acid solution, continue to pass carbon dioxide gas flow under the liquid surface for protection, quickly and accurately add 45mL of potassium dichromate standard titration solution, then titrate with the titanium nitride standard titration solution to be calibrated to the end point close to the calculated amount, immediately add 25mL of ammonium thiocyanate solution, and continue to titrate with the titanium chloride standard titration solution to be calibrated until the red color turns to green, which is the end point. The entire titration process should be operated under the protection of carbon dioxide gas flow, and at the same time, use 45mL of water instead of potassium dichromate solution to do a blank test in the same way.
A3.3 Expression of the concentration of titanium trichloride standard titration solution The concentration of titanium trichloride standard titration solution (c) is calculated according to formula (A1): V,xci
(Al)
Wherein: V,--the volume of potassium dichromate standard titration solution, mL;--the volume of titanium trichloride standard titration solution consumed by the potassium dichromate standard titration solution oxidized to high iron, mL; Va
the volume of titanium trichloride standard titration solution consumed in the titration blank, mL: Va
the actual concentration of potassium dichromate standard titration solution, mal/L. Note: The above calibration needs to be performed immediately when analyzing the sample. 4270002g, placed in a 500mL conical flask, under the protection of carbon dioxide gas flow, add 50mL of freshly boiled and cooled water to dissolve it, then add 25mL of sulfuric acid solution, continue to pass carbon dioxide gas flow under the liquid surface for protection, quickly and accurately add 45mL of potassium dichromate standard titration solution, then titrate with the titanium nitride standard titration solution to be calibrated to the end point close to the calculated amount, immediately add 25mL of ammonium thiocyanate solution, and continue to titrate with the titanium chloride standard titration solution to be calibrated until the red color changes to green, which is the end point. The entire titration process should be operated under the protection of carbon dioxide gas flow, and at the same time, use 45mL of water instead of potassium dichromate solution to do a blank test in the same way.
A3.3 Expression of the concentration of titanium trichloride standard titration solution The concentration of titanium trichloride standard titration solution (c) is calculated according to formula (A1): V,xci
(Al)
Wherein: V,--the volume of potassium dichromate standard titration solution, mL;--the volume of titanium trichloride standard titration solution consumed by the potassium dichromate standard titration solution oxidized to high iron, mL; Va
the volume of titanium trichloride standard titration solution consumed in the titration blank, mL: Va
the actual concentration of potassium dichromate standard titration solution, mal/L. Note: The above calibration needs to be performed immediately when analyzing the sample. 4270002g, placed in a 500mL conical flask, under the protection of carbon dioxide gas flow, add 50mL of freshly boiled and cooled water to dissolve it, then add 25mL of sulfuric acid solution, continue to pass carbon dioxide gas flow under the liquid surface for protection, quickly and accurately add 45mL of potassium dichromate standard titration solution, then titrate with the titanium nitride standard titration solution to be calibrated to the end point close to the calculated amount, immediately add 25mL of ammonium thiocyanate solution, and continue to titrate with the titanium chloride standard titration solution to be calibrated until the red color changes to green, which is the end point. The entire titration process should be operated under the protection of carbon dioxide gas flow, and at the same time, use 45mL of water instead of potassium dichromate solution to do a blank test in the same way.
A3.3 Expression of the concentration of titanium trichloride standard titration solution The concentration of titanium trichloride standard titration solution (c) is calculated according to formula (A1): V,xci
(Al)
Wherein: V,--the volume of potassium dichromate standard titration solution, mL;--the volume of titanium trichloride standard titration solution consumed by the potassium dichromate standard titration solution oxidized to high iron, mL; Va
the volume of titanium trichloride standard titration solution consumed in the titration blank, mL: Va
the actual concentration of potassium dichromate standard titration solution, mal/L. Note: The above calibration needs to be performed immediately when analyzing the sample. 427
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