Some standard content:
GB 4481.1—1999
This standard is not equivalent to the 6th edition of the Japanese Food Additive Code (1992). GB4481.1—1994 was revised based on the "Edible Yellow No. 4 (Tartrazine)" standard in the book. The main 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 content index of water-insoluble matter in this standard is ≤0.30%, while the index of the Japanese standard is ≤0.20%. 3. The total amount of drying loss, chloride (calculated as NaCl) and sulfate (calculated as Na2SO.) in the tartrazine 85 specification in this standard is ≤15.0%; the Japanese index The content of heavy metals (in terms of Pb) in this standard is ≤0.001%, and the content of Japanese heavy metals (in terms of Pb) is ≤0.002%. 5. The content of secondary dyes in this standard is determined in accordance with GB4481.1-1994, and the determination method in FAO/WHO is adopted, with the index of 10%.
6. The content of arsenic in this standard is determined in accordance with the determination method in GB/T8450-1987 Food Additives, with the index of ≤0.0001% (in terms of As), and the Japanese index is ≤0.00 4% (As203). 7. In addition to the titanium trichloride titration method, this standard adds a relatively simple spectrophotometric method for content determination for daily determination. The titanium trichloride method is used as the arbitration method.
8. The determination method for fluoride (measured in NaCl) and sulfate (measured in Na?SO4) in this standard is chemical titration, while the Japanese standard uses ion chromatography.
The main differences between this standard and GB4481.1-1994 are as follows: 1. GB4481.1-1994 has two specifications of lemon yellow 85 and lemon yellow 60. This standard lemon yellow 60 is the reserved specification. 2. This standard adds chloride (measured in NaCl) and sulfate (measured in Na2SO.) content determination to the lemon yellow 85 specification, and combines chloride (measured in NaCl) and sulfate (measured in Na2SO.) and drying loss items into the total amount, with an index of ≤1 5.0%. 3. Cancel the determination of isocyanate extract content. 4. The rest are the same as GB4481.1-1994. This standard was first issued in 1984 and revised for the second time in 1999. This standard will replace GB4481.1-1994 from the date of implementation. Appendix A in this standard is the appendix of the standard. This standard was proposed by the State Bureau of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Technical Committee on Standardization of Dyes 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 Institute of the Shanghai Municipal Health Bureau. The main drafters of this standard are: Ding Deyi, Liu Jing, Shi Huaijiong, Ying Huiru, Guan Jianxiong, Zhou Yanqin. This standard is entrusted to the National Technical Committee on Standardization of Dyes for interpretation. 379
National Standard of the People's Republic of China
Food Additives
Tartrazine
Food additive-
Tartrazine
GB4481.1--1999
Replaces GB 4481.1-1994
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of food additive tartrazine. This standard is applicable to dyes formed by the condensation of dihydroxytartaric acid and phenylhydrazine p-sulfonic acid, or the coupling of p-aminobenzenesulfonic acid with 1-(4-sulfophenyl)-3-carboxylpyrazolone-5 after diazotization.
Structural formula:
Molecular formula: ChH, N, Na.O, S2
Relative molecular mass: 534.37 (according to the 1995 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard by reference in this standard. When this standard was published, the versions shown were all valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest version of the following standards. GB/T601—1988 Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) Chemical reagents
GB/T 602—1988
Preparation of standard solutions for impurity determination
GB/T603—1988 Chemical reagents
Preparation of preparations and products used in test methods GB/T6682-
2—1990
GB/T 8450—1987
3 Requirements
Specifications and test methods for water used in analytical laboratories Determination of monuments in food additives
3.1 Appearance Orange-yellow powder.
3.2 The quality of food additive lemon yellow 85 should meet the requirements of Table 1. Approved by the State Administration of Quality and Technical Supervision on July 12, 1999 380
Implementation on January 1, 2000
GB 4481. 1—1999
Loss on drying, total amount of chloride (as NaCl) and sulfate (as Na?SO,) Water-insoluble matter
Secondary dyes
Arsenic (as As)
Heavy metals (as Ph)
3.3 The quality of food additive Tartrazine 60 shall comply with the requirements of Table 2. Tartrazine 60 is a reserved specification. Table 2 Requirements
Loss on drying
Insoluble matter in water
Subsidiary dye
Monument (in terms of As)
Heavy metal (in terms of Pb)
Note: The reserved specifications are those that are restricted in development and to be cancelledTest methods
The reagents and water used in this standard, unless otherwise specified, refer to analytical 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, T 602 and GB/T603 unless otherwise specified.
4.1 Appearance
Measured by visual inspection.
4.2 Identification
4.2.1 Reagents and materials
a) Sulfuric acid solution: 1+100;
b) Ammonium acetate solution: 1.5g/1.
4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Test method
4.2.3.1 Weigh about 0.1g of the sample and dissolve it in 100mL of water to produce a yellow clear solution. 4.2.3.2 Take 40mL of the yellow solution in 4.2.3.1, add 10mL of sulfuric acid solution and the solution will turn yellow. Take 2~3 drops of this solution and add it to 5mL of water to produce a yellow color.
4.2.3.3 Weigh 0.1g of the sample and dissolve it in 100mL of ammonium acetate solution. Take 1mL of this solution and add ammonium acetate solution to make it 100nl. The maximum absorption wavelength of the solution is 428nm±2nm. 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 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:
GB 4481. 1-- 1999
b) Titanium trifluoride standard titration solution c (TiCl3) = 0.1 mol/L (newly prepared, see Appendix A for preparation method) c) Carbon dioxide in cylinders.
4.3.1.3 Test method
Weigh 5 g of lemon yellow 85 or lemon yellow 60 sample, accurate to 0.0002 g, dissolve it in 100 ml of water that has been freshly boiled and cooled to room temperature, transfer it to a 500 mL volumetric flask, dilute to the scale, shake the hook, accurately pipette 50 mL, place it in a 500 mL conical flask, add 15 g of sodium hydrogen tartrate + 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.
1--shaped bottle (500mL); 2-brown burette (50 mL), 3-lower-mouthed glass bottle wrapped in black paper (2000ml); 4-container for a mixture of 10% ammonium carbonate and 10% ferrous sulfate (5000mL); 5-piston; 6-empty bottle; 7-washing bottle filled with water
Figure 1 Apparatus diagram of titanium trichloride titration
4.3.1.4 Expression of analytical results
Express the content of lemon yellow in mass percentage (X,) according to formula (1): X = ×c × 9.1336 × 100 =
VX e X 133.6
m×500
Wherein: V
The volume of titanium trifluoride standard titration solution consumed for titration of sample, mL: The actual concentration of titanium trichloride standard titration solution, mol/L The mass of sample·g:
（1）
The mass of lemon yellow in grams equivalent to 1.00mL titanium trichloride standard titration solution [c(TiCl:)=1.000mol/L].
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 Method summary
GB 4481: 1 1999
Dissolve the sample and the standard sample with known content in water respectively, measure their absorbance at the maximum absorption wavelength, and then calculate the content of the sample.
4.3.2.2 Reagents and materials
Standard sample of lemon yellow 85 or lemon yellow 60: homemade·The content is determined by titration with titanium trifluoride. 4.3.2.3 Instruments and equipment
a) Spectrophotometer;
b) Colorimetric III: 10 mm.
4.3.2.4 Preparation of standard solution of lemon yellow 85 or lemon yellow 60 Weigh 0.5g of standard sample of lemon yellow 85 or lemon yellow 60, accurate to 0.0002g, dissolve in appropriate amount of water, transfer to a 1000ml volumetric flask, dilute to scale, and shake to hook. Accurately pipette 10mL, transfer to a 500mL volumetric flask, dilute to scale, and shake to hook. 4.3.2.5 Preparation of sample solution of lemon yellow 85 or lemon yellow 60 Weigh 0.5g of sample, and the rest is the same as the preparation of standard solution. 4.3.2.6 Test method
Put the standard solution and sample solution in 10mm colorimetric solution, and measure the absorbance of each at a wavelength of 428nm±2nm using a spectrophotometer.
Use water as the reference solution.
4.3.2.7 Expression of analysis results
Express the content of tartrazine in mass percentage (X,) and calculate it according to formula (2): X,=
Wherein: A—absorbance of sample solution:
A. absorbance of standard solution;
X.—mass percentage of tartrazine standard sample (titanium chloride method). 4.3.2.8 Allowable error
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, total amount of chloride (as NaCl) and sulfate (as Na2SO4) 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 weighing bottle of (30-40) mm that has been weighed to a constant weight, and dry in a constant temperature oven at 135°C ± 2°C to constant weight.
4.4.1.2 Expression of analysis results
Express the loss on drying content (X:) in mass percentage and calculate according to formula (3): Xsm=m×100
Where: m2——mass of sample before drying,; ml——mass of sample after drying to constant weight, g. 4.4.1.3 Permissible 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;
GB 4481.1-1999
d) Silver nitrate standard titration solution: c(AgNO:)=0.1mol/Le) Ammonium thiocyanate standard titration solution: c(VH,CNS)=0.1mo1/L, 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 sample (lemon yellow 85) to the nearest 0.001g, add 200mL of water, 10g of activated carbon, and 1mL of nitric acid solution, stir evenly, place for 30min (stir occasionally) and filter with dry filter paper. If the filtrate is colored, add 2g of activated carbon and place for 1h under occasional stirring, 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
Take 50mL of the above test solution and 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 test solution and titrate with ammonium thiocyanate standard titration solution until the solution turns brick red, which is 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 according to formula (4): x = VV)× 0 058 4 × 100 V.-V)×c× 23 36m×200
The volume of ammonium thiocyanate standard titration solution consumed in the titration of the sample, mL; Wherein: V-—
The volume of ammonium thiocyanate standard titration solution consumed in the titration of the blank solution, mL; the actual concentration of the ammonium thiocyanate standard titration solution, mol/L; the mass of the sample, g;
(4))
0.0584——The mass of sodium chloride in grams equivalent to 1.00mL of ammonium thiocyanate standard titration solution [Lc(NH,CNS)=1.000mol/L], nom.
4.4.2.5 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.3%, and the arithmetic mean shall be taken as the determination result. 4.4.3 Determination of sulfate (in terms of Na, SO.) 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) Tetrahydroxybenzoic acid disodium-potassium chloride mixed indicator: mixed in equal amounts; f) Sulfuric acid standard solution: c (1/2H,S O,) = 0.1mal/L; g) Phenolic acid indicator solution: 10g/L;
h) Sodium rose bengalate indicator solution: weigh 0.1g of sodium rose bengalate. Dissolve in 10mL of water (prepare and use immediately) i) Barium chloride standard titration solution: c (1/2BaCl) = 0.1mol/L; Preparation: weigh 12.25g of sodium chloride, dissolve in 500mL of water, transfer to a 1000mL volumetric flask, dilute to the scale, and shake well. Calibration: absorb 20mL of sulfuric acid standard solution, add 50mL of water, and neutralize with ammonia water until the bright yellow test paper shows an alkaline reaction, then titrate with barium chloride standard solution, use sodium rose bengalate indicator solution as an extra-liquid indicator, and the end point is when a rose-red spot appears on the filter paper and remains unchanged for 2 minutes.
The concentration of the barium chloride standard titration solution (X.) is calculated according to formula (5): XWww.bzxZ.net
GB 4481. 1-1999
Wherein: V is the volume of the standard sulfuric acid titration solution, mLV, — is the volume of the standard barium chloride titration solution, mL; — is the actual concentration of the standard sulfuric acid titration solution, mol/l. 4.4.3.2 Test method
Pipette 25 mL of the test solution and place it in a 250 mL conical flask, add 1 drop of phenol anhydride indicator solution, add sodium hydroxide solution to turn pink, then add hydrochloric acid solution until the pink color disappears, then add 30 mL of ethanol and 0.4 g of tetrahydroxybenzoic acid disodium-potassium chloride mixed indicator, shake the hook, and after dissolving, titrate the barium chloride standard solution with continuous shaking until the solution turns rose red as the end point. During the titration, use a light to illuminate from the side for careful observation, and use rose red sodium acid indicator solution as an external indicator for comparison. At the same time, perform a blank test in the same way. 4.4.3.3 Expression of analysis results
Express the content of sulfate (in terms of Na2SO4) in mass percentage (X2). Calculate according to formula (6): X2 = (V-V) × c × 0.071
(V-V) × c × 56.8
Wherein: V—the volume of barium chloride standard titration solution consumed in titrating the sample solution, mL; V—the volume of barium chloride standard titration solution consumed in titrating the blank solution, mL; r—the actual concentration of barium chloride standard titration solution, mol/L; m—the mass of the sample + g;
0.071—the mass of sodium sulfate in grams equivalent to 1.00 mL of barium chloride standard titration solution [Lc(1/2BaCl2) = 1.000 mol/L] + g.
4.4.3.4 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. 4.4.4. Expression of analytical results
The content of loss on drying expressed in mass percentage The sum of the content of chloride (in terms of NaCl) and the content of sulfate (in terms of Na2SO4) (X3) is calculated according to formula (7):
X3 -X+X3+X3
Wherein: X3 — the content of loss on drying expressed in mass percentage; X3 — the content of chloride expressed in mass percentage; X3 — the content of sulfate expressed in mass percentage. 4.5 Determination of water-insoluble matter
4.5.1 Determination method
Weigh about 3g of sample to an accuracy of 0.01g, place it in a 500mL beaker, add 250mL of 50℃~60℃ water to dissolve it, filter it through a No. 4 glass sand core crucible that has been dried to constant weight at 135℃±2℃, and wash it thoroughly with hot water until the washing liquid is colorless, and dry it in a constant temperature oven at 135℃±2℃ to constant weight.
4.5.2 Expression of analysis results
Express the content of water-insoluble matter (X.) in mass percentage according to formula (8): Xs=\×100
Where: m:——mass of water-insoluble matter after drying, g; mass of sample·g.
4.5.3 Permissible 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 Summary of method
GB 4481. 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;
c) Acetone solution: 1-1;
d) Ammonia solution: 4+96;
e) Sodium bicarbonate solution: 4g/L,
4.6.3 Instruments and equipment
a) Spectrophotometer;
b) Chromatography filter paper: No. 1 medium speed, 150mm×250mmc) Chromatography cylinder: $240mmX300mm:
d) Microinjector: 100μl
4.6.4 Test method
4.6.4.1 Paper chromatography conditions
a) Developing solvent: n-butanol + deca-anhydrous ethanol + deca-ammonia solution = 6+2-3; b) Temperature: 20C～25℃.
4.6.4.2 Preparation of sample eluate
Weigh 1g of lemon yellow 85 or lemon yellow 60 sample, accurate to 0.01g, and place it in a beaker. Add appropriate amount of water to dissolve it, then transfer it to a 100mL volumetric flask, dilute to the mark, shake well, and use a micro-injector to draw 200μuL, evenly spot it on a baseline 25mm away from the bottom edge of the filter paper, in 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 developing agent. Wait until the front line of the developing agent rises to 150mm or until the secondary dye is separated satisfactorily (see Figure 2). Take out the chromatography filter paper and blow it with cold air from a hair dryer. 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 filter paper used for developing the test solution on the same 600mmX600mm filter paper). 150mm
Subsidiary dye
Main dye
Figure 2 Schematic diagram of secondary dye chromatography
GB 4481. 1-1999
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 thin strips of about mm×15mm, put them in a 50mL Nessler colorimetric tube, accurately add 5mL of acetone solution, shake for 3min~5min, then accurately add 20mL of sodium bicarbonate solution and shake thoroughly, filter the extracts naturally in No. 3 glass sand core funnels, the filtrate must be clear and free of suspended matter, and measure the absorbance on a spectrophotometer at the maximum absorption wavelength of the secondary dye using a 50mm colorimetric dish. Use a mixture of 5ml of acetone solution and 20mL of sodium bicarbonate solution as the reference solution. 4.6.4.3 Preparation of standard eluate
Pipette 2mL of the above 1% sample solution, transfer to a 100mL volumetric flask, dilute to the mark, and shake well. 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, put the filter paper in the chromatography tank for development, wait until the front line of the developing agent rises only 40mm, take it out and blow it dry, cut off all the dye parts, and perform the extraction operation as before. Use a 10mm colorimetric dish to measure the absorbance at the maximum absorption wavelength.
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 in lemon yellow 85 in mass percentage (X.) and calculate according to formula (9): A-6
×2×0
X,= A = b,
Absorbance of accessory dye extract calculated at a light path length of 50 mm: Wherein: A—absorbance of accessory dye control blank extract calculated at a light path length of 50 mm; h
A—absorbance of standard extract calculated at a light path length of 10 mm; b,——-absorbance of standard control blank extract calculated at a light path length of 10 mm; 5—the ratio converted to the value calculated at a light path length of 10 mm; 2—reference concentration of standard extract based on 1% sample solution, %; 85
total content of the sample.
To express the secondary dye content in lemon yellow 60 in mass percentage, 85/100 in the above formula should be changed to 60/100. 4.6.4.5 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. 4.7 Determination of monument content
4.7.1 Reagents and materials
a) Nitric acid;
b) Sulfuric acid solution: 1-1;
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 of arsenic (As) in a 100mL volumetric flask and dilute to the scale.
4.7.2 Instruments and equipment
The device of the arsenic spot method in GB/T8450-1987. 4.7.3 Test method
Weigh 1g of lemon yellow 85 or lemon 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 over low heat to drive out nitrogen dioxide gas. When the solution turns brown, stop heating. Let it cool and add 5ml of nitric acid-perchloric acid mixture. Heat over high heat until the solution is transparent, colorless or slightly yellow. If it is still opaque, let it cool and add 5ml of nitric acid-perchloric acid mixture. Continue heating until the solution is clear, colorless or slightly yellow and produces white smoke. Stop heating, let it cool and add 5ml of water and heat to boiling to remove residual nitric acid-perchloric acid (add water and boil it again if necessary). Continue heating until white smoke is produced and keep for 10min. Let it cool and transfer it to a 100ml conical flask. The following shall be carried out in accordance with the provisions of 2.4 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;
f) Sodium sulfide solution: 100g/L
GB 4481.1-1999
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 mark.
4.8.2 Preparation of sample solution
Weigh 2.5g of lemon yellow 85 or lemon yellow 60 sample, accurate to 0.01, place in a crucible made of platinum (or quartz, porcelain), add a small amount of sulfuric acid to moisten, slowly burn, try to make it almost completely ash at low temperature, then add 1mL of sulfuric acid, gradually heat until sulfuric acid gas is almost no longer generated. Put it in an electric furnace, burn at 450℃~550C until it is ash, then cool it. Add 3mL of hydrochloric acid and shake well, then add 7ml of water and shake well. Filter 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 liquid and the filtrate, 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 sample solution, put it into 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 Nessler colorimetric tube, add 2.0ml of lead standard solution.and 1 drop of phenolic acid indicator solution, prepared 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 Lemon Yellow 85 or Lemon Yellow 60 in accordance with the provisions of this standard. The production unit shall ensure that the quality of all food additives Lemon Yellow 85 or Lemon Yellow 60 shipped from the factory meets the requirements of this standard and has a quality certificate in a certain format.
5-2 The food additive Lemon Yellow 85 or Lemon Yellow 60 is a batch of uniform products mixed at one time. 5.3 For bottled products, 10% of the total number of product packaging boxes (each box is 10×0.5kg) should be selected. Then 10% of the bottles should be selected from the selected boxes. From the selected bottles, take out no less than 50 samples 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 about 100g from them. Put them in two clean and 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 additives Lemon Yellow 85 or Lemon 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. 388
GB4481.1--1999
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 label number and label name, shelf life, production date and batch number, net content, and instructions for use. 6.3 Food additives Lemon Yellow 85 or Lemon Yellow 60 are packed in polyethylene plastic bottles, 0.5kg per bottle, and every 10 bottles are sealed in a box. Other forms of packaging can be determined by negotiation between the manufacturer and the user. 6.4 During transportation, it must be protected from rain, moisture, and sunlight, 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 storage and transportation. 6.6 The shelf life of this product is five years from the date of production. It can only be used if it is re-inspected after the expiration date and fully complies with the requirements of this standard. 389
A1 Reagents and materials
a) Hydrochloric acid:
b) Ammonium ferrous sulfate;
c) Ammonium thiocyanate solution: 200g/L;
d) Sulfuric acid solution: 1+1;
GB 4481.1—1999
Appendix A
(Appendix to the standard)
Preparation method of titanium trichloride standard titration solutione) Potassium dichromate standard titration solution: c1/6K,Cr,O,)=0.1mol/L. A2 Instruments and equipment
See Figure 1.
3 Preparation of titanium trichloride standard titration solution
A3.1 Preparation
Take 100 ml of titanium trichloride solution and 75 ml of hydrochloric acid, place them in a 1000 ml brown volumetric flask, dilute to the scale with freshly boiled water that has been cooled to room temperature, shake well, pour immediately 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 chain bottle. 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 trichloride 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 trichloride standard titration solution to be calibrated until the red color changes to green, which is the end point. The entire titration process should be carried out 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 by formula (A1): Vixc
Wherein: V. Volume of potassium dichromate standard titration solution, mLA1)
V2—…-The volume of titanium trichloride standard titration solution consumed by the potassium dichromate standard titration solution to oxidize into high iron, mL.; Vs—The volume of titanium trichloride standard titration solution consumed by the titration blank, mL: c The actual concentration of potassium dichromate standard titration solution, mol/L. Note: The above calibration needs to be performed immediately when analyzing the sample. 3900002g, placed in a 500mL chain bottle, 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 trichloride 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 trichloride 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 by formula (A1): Vixc
Wherein: V. Volume of potassium dichromate standard titration solution, mLA1)
V2—…-The volume of titanium trichloride standard titration solution consumed by the potassium dichromate standard titration solution to oxidize into high iron, mL.; Vs—The volume of titanium trichloride standard titration solution consumed by the titration blank, mL: c The actual concentration of potassium dichromate standard titration solution, mol/L. Note: The above calibration needs to be performed immediately when analyzing the sample. 3900002g, placed in a 500mL chain bottle, 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 trichloride 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 trichloride 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 by formula (A1): Vixc
Wherein: V. Volume of potassium dichromate standard titration solution, mLA1)
V2—…-The volume of titanium trichloride standard titration solution consumed by the potassium dichromate standard titration solution to oxidize into high iron, mL.; Vs—The volume of titanium trichloride standard titration solution consumed by the titration blank, mL: c The actual concentration of potassium dichromate standard titration solution, mol/L. Note: The above calibration needs to be performed immediately when analyzing the sample. 390
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