Some standard content:
GB4479.11999
This standard adopts the 6th edition of the Japanese Food Additives Standard (1992) in a non-equivalent manner. GB4479.1-1996 was revised according to the standard "Edible Red No. 2 (Amaranth Red)" 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 content index of water-insoluble matter in this standard is ≤0.30%, while the index of Japan is ≤0.20%. 3. The total amount of drying loss, chloride (calculated as NaCl) and sulfate (calculated as Na?SO.) in the specification of Amaranth Red 85 in this standard is ≤15.0%, while the Japanese standard is listed as drying loss index ≤10.0%, chloride and sulfate index ≤5.0%. 4. The content index of heavy metals (in terms of Pb) in this standard is ≤0.001%, and the index in Japan is ≤0.002%. 5. The content of secondary dyes in this standard is determined by GB4479.11996, using the determination method in FAO/WHO, and the index is ≤3. 0%.
6. The content of arsenic in this standard is determined by the determination method in GB/T8450 Food Additives, and the index is ≤0.0001% (in terms of As), and the index in Japan is ≤0.0004% (As20). 7. 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.
8. The determination method of chloride (in terms of NaCl) and sulfate (in terms of Na2SO4) in this standard is chemical titration, and the Japanese standard adopts ion chromatography.
The main differences between this standard and GB4479.1-1996 are as follows: 1. GB4479.1-1996 has two specifications: Amaranth 85 and Amaranth 60. Amaranth 60 in this standard is the reserved specification. 2. In the Amaranth 85 specification of this standard, the drying loss, fluoride (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 GB4479.1-1996.
This standard was first issued in 1986 and revised for the second time in 1999. From the date of implementation, this standard will replace GB4479.1--1996. 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 the Shanghai Dye Research Institute and the Health Supervision Institute of the Shanghai Municipal Health Bureau. The main drafters of this standard are Ding Deyi, Liu Jing, Shi Huaijiong, Cheng Chunhong, Guan Jianxiong and Zhou Yanqin. This standard is entrusted to the National Technical Committee on Dye Standardization for interpretation. 339
1 Scope
National Standard of the People's Republic of China
Food additive
Amaranth
Food additive
Amaranth
GB 4479. 1—1999
Replaces GB4479.1—1996
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation and storage of the food additive amaranth. This standard applies to dyes obtained by coupling 1-aminonaphthalene-4-sulfonic acid with sodium 2-naphthol 3,6-disulfonate after diazotization. Structural formula:
Molecular formula C2.HN, NaaOioS3
Relative molecular mass: 604.48 (according to the 1995 international relative atomic mass) Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid, all standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601--1988 Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) GB/T 602--1988
GB/T 603-1988
Preparation of standard solutions for determination of impurities
Chemical reagents
Preparation of preparations and products used in chemical reagent test methods GB/T 6682-1992
GB/T 8450-1987
3 Requirements
Specifications and test methods for water used in analytical laboratories Determination of arsenic in food additives
3.1 Appearance This product is a reddish brown to dark reddish brown powder. 3.2 The quality of food additive Kuancaihong 85 should meet the requirements of Table 1. Approved by the State Administration of Quality and Technical Supervision on July 12, 1999 340
Implementation on January 1, 2000
GB 4479. 1- 1999
Requirements in Table 1
Loss on drying, total amount of chloride (as NaCl) and sulfate (as Na2SO4) Water-insoluble matter
Secondary dyes
Arsenic (as As)
Heavy metals (as Pb)
3 The quality of food additive Amaranth 60 shall comply with the requirements of Table 2. Kuanlai Red 60 is a reserved specification. 3.3
Requirements of Table 2
Loss on drying
Water insoluble matter
Subsidiary dye
Arsenic (measured in As)
Heavy metal (measured in Pb)
Note: Reserved specifications are those that are restricted in development and are to be cancelled. 4 Test 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/T602 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/L.
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. A clear red solution with purple light will appear. 4.2.3.2 Take 40 mL of the clear red solution with purple light in 4.2.3.1, add 10 mL of sulfuric acid solution, the solution turns purple, take 2~3 drops of this solution and add 5 mL of water, a red solution with purple light appears, 4.2.3.3 Weigh 0.1 g of the sample, dissolve it in 100 mL of ammonium acetate solution, take 1 mL of this solution and add ammonium acetate solution to 100 nL, the maximum absorption wavelength of the solution is 520 nm ± 2 nm. 4.3 Determination of content
4.3.1 Titanium trichloride titration method (arbitration method) 4.3.1.1 Summary of the method
GB 4479.1-1999
In a neutral medium, the azo group in the sample is reduced and decomposed by titanium trichloride, and the percentage of the dye is calculated according to the consumption of titanium trichloride standard titration solution.
4.3.1.2 Reagents and materials
a) Trisodium citrate:
b) Standard titration solution of trichloride c(TiCl) = D.1 mol/I (freshly prepared. See Appendix A for preparation method): c) Carbon dioxide in a cylinder.
4.3.1.3 Test method
Weigh 5g of the sample of Yuancaihong 85 or Kuancaihong 60, dilute to 0.0002g, dissolve in 100ml of freshly boiled and cooled water, transfer to a 500mL volumetric flask, dilute to volume, shake well, and pipette 50mL, place in a 500mL conical flask, add 15g of trisodium citrate and 150mL of water, assemble the instrument according to Figure 1, heat to boiling while passing carbon dioxide gas below the liquid surface, and titrate with standard titration solution of titanium trichloride until colorless as the end point.
1-conical flask (500ml); 2-brown burette (50mL); 3-bottomed glass bottle wrapped with black paper [2000mL); 4-container containing equal amounts of 10% ammonium carbonate and 10% ferrous sulfate coagulation solution (5000mL); 5-piston; 6-empty bottle; 7-washing bottle filled with water
Figure 1 Apparatus diagram of titanium trichloride titration method
4.3.1.4 Expression of analytical results
The content of amaranth red expressed as mass percentage (X,) is calculated according to formula (1): X, =YXc×0.1511×100 =VXcX151.1×50
Wherein: V is the volume of titanium trichloride standard titration solution consumed for titrating the sample, ml; the actual concentration of titanium trioxide standard titration solution, mol/.; V is the mass name of the sample;
(1)
and 1.00mL titanium trioxide standard titration solution [c (TiC1,) = 1.000mol/L equivalent to 0.151 1-
mass of amaranth expressed in grams +:
4.3.1.5 Permissible 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. 342
4.3.2 Spectrophotometric colorimetry
GB 4479. 1-1999
4.3.2.1 Method summary
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
Amaranth 85 or Amaranth 60 standard sample: homemade, content determined by titanium trichloride titration. 4.3.2.3 Instruments and equipment
a) Spectrophotometer:
b) Colorimetric III: 10 mm.
4.3.2.4 Preparation of Amaranth 85 or Amaranth 60 standard sample solution Weigh 0.5g of Amaranth 85 or Amaranth 60 standard sample to an accuracy of 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 Amaranth Red 85 or Amaranth Red 60 test solution Weigh 0.5g of the sample and prepare the rest in the same way as the standard solution. 4.3.2.6 Test method
Place the standard solution and the sample solution in a 10mm cuvette and measure the absorbance of each at a wavelength of 520nm±2nm using a spectrophotometer.
Use water as the reference solution.
4.3.2.7 Expression of analysis results
Express the content of Amaranth Red 85 or Amaranth Red 60 in mass percentage (X) according to formula (2): X2
Where: A——absorbance of the sample solution: A
A.—absorbance of the standard solution;
X——mass percentage of Amaranth Red 85 or Amaranth Red 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 loss on drying, total amount of chloride (calculated as NaCl) and sulfate (calculated as Na2SO4.4.7 Determination of loss on dryingwww.bzxz.net
(2))
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 until constant weight.
4.4.1.2 Expression of analysis results
Express the drying loss content (X:) in mass percentage according to formula (3): X,=m2=m × 100
wherein m-
mass of the sample before drying·g
mass of the sample after drying to constant weight·.
4.4.1.3 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;
GB 4479. 1-- 1999
d) Silver nitrate standard titration solution: c(AgNO,)=0.1mol/L; e) Ammonium thiocyanate standard titration solution: c(VH,CNS)=0.1mol/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 Amaranth 85 sample, accurate to 0.001g, add 200mL of water, add 10g of activated carbon, and then add 1mL of nitric acid solution, stir evenly, let it stand for 30min (stir occasionally during this period), filter with dry filter paper, if the filtrate is colored, add 2g of activated carbon, stir occasionally and let it stand 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 fluoride 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) according to formula (4): (Vi-V)XcX0. 0584×100=X
(Vi-V)×cX23.36
Wherein: V——the volume of ammonium thiocyanate standard titration solution consumed in titrating the sample, mL; V,—the volume of ammonium thiocyanate standard titration solution consumed in titrating the blank solution, mL; the actual concentration of the ammonium thiocyanate standard titration solution, mal/L; ....(4)
m—mass of sample·g;
0.0584—the mass of sodium oxide in grams equivalent to 1.00mL of ammonium thiocyanate standard titration solution [c(NH,CNS)=1.000mol/L]+g.
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 (as NazSO.) content 4.4.3.1 Reagents and materials
a) Ammonia water:
b) Sodium hydroxide solution: 0.2g/Lt
c) Hydrochloric acid solution: 1+99;
d) Ethanol: 95%:
e) Tetrahydroxybenzoic acid disodium-potassium chloride mixed indicator: mixed in equal amounts: f) Standard sulfuric acid titration solution: c(1/2H SO4)=0.1mol/Lg) Phenol indicator solution: 10g/L;
h) Sodium rose bengalate indicator solution: weigh 0.1g sodium rose bengalate and dissolve it in 10mL water (prepare and use immediately);i) Standard titration solution of barium chloride: c(1/2BaCl2)=0.1mol/L;-Preparation: weigh 12.25g barium chloride, dissolve it in 500mL water, transfer it into 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 it with hydrogen water until the bright yellow test paper shows alkaline reaction, then titrate with standard fluoride solution, use sodium rose bengalate indicator solution as extra-liquid indication, and the end point is when a rose-red spot appears on the filter paper and remains unchanged for 2min.
In the formula: V
GB 4479.1—1999
The concentration of the standard titration solution of barium chloride (X,) is calculated according to formula (5): X.
The volume of the standard titration solution of sulfuric acid, mL;
V,The volume of the standard titration solution of barium chloride, mL; xc
The actual concentration of the standard titration solution of sulfuric acid, mol/L. 4.4.3.2 Test method
(5)
Take 25mL of the test solution and place it in a 250mL 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 30mL of ethanol and 0.4g of tetrahydroxybenzene disodium ether-potassium chloride mixed indicator. Shake well, and after dissolving, titrate with barium chloride standard solution under continuous shaking until the solution turns rose red as the end point. During the titration, use light to illuminate from the side and observe carefully. Use sodium rose red 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 analytical results
Express the content of sulfate (in terms of Na2SO) in mass percentage (X). Calculate according to formula (6): X.
Where: V
(V - Vi) X c X 0. 071 × 200×100
(V - V) X c X 56. 8
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, mal/L...(6)
The mass of the sample, g;
The mass of sodium sulfate in grams equivalent to 1.00mL barium chloride standard titration solution c (1/2BaCl.) = 1.000mal/LJ, 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 sum of the content of dry weight loss, the content of chloride (in terms of NaCl) and the content of sulfate (in terms of Na2SO4) expressed in mass percentage (X,) is calculated according to formula (7):
X, X+X+ X
Wherein: X, — the content of dry weight loss expressed in mass percentage, %; X. — the content of chloride expressed in mass percentage, %; X. — the content of sulfate expressed in mass percentage, %. 4.5 Determination of water-insoluble matter content
4.5.1 Test method
Weigh about 3g of sample to the nearest 0.01g, place it in a 500mL beaker, add 250mL of 50C~60C water to dissolve it, filter it through a No. 4 glass sand core 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 (Xg) in mass percentage. Calculate according to formula (8): Xg=ma × 100
Where: m3——the mass of water-insoluble matter after drying B+2
the mass of the sample, g.
4.5.3 Permissible difference
GB 4479. 1-1999
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
The components are separated and eluted by paper chromatography, and then quantified 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) Chromatographic filter paper: No. 1 medium speed, 150mm×250mm; r) Chromatographic cylinder: $240mm×300mm;
d) Micro-injector: 100μl.
4.6.4 Test method
4.6.4.1 Paper chromatography conditions
a) Developing solvent: n-butanol + anhydrous ethanol → ammonia solution = 6+2+3; b) Temperature: 20C~25℃.
4.6.4.2 Preparation of sample eluate
Weigh 1g of Amaranth 85 or Amaranth 60 sample + accurate to 0.01g and place in a beaker, add appropriate amount of water to dissolve, transfer to a 100mL volumetric flask, dilute to scale, shake, use a micro-injector to draw 200μL evenly 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 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. When the front line of the developing agent rises to 150mm or until the secondary dye is separated satisfactorily, take out the chromatography filter paper and blow dry 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 (1)
Subsidiary dye (2)
Subsidiary dye (3)
Ketone dye
Subsidiary dye (4)
Figure 2 Schematic diagram of subsidiary dye chromatography
GB 4479. 1 -- 1999
Cut each subsidiary dye and the filter paper at the corresponding position on the blank filter paper to the same size, and cut into thin strips of about 5mm×15mm. Place them in 50mL Nessler colorimetric tubes respectively, accurately add 5mL of acetone solution to each, shake for 3min~5min, then accurately add 20mL of sodium bicarbonate solution and 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 dishes to measure the absorbance on a spectrophotometer at the maximum absorption wavelength of each subsidiary 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 well. Use a microinjector 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 cuvette.
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 dyes in mass percentage (X,) according to formula (9): (A,-b) + ..* +(A,-b.)
Wherein: A1,, A,-absorbance of each accessory dye extract calculated at 50mm optical path length; b++**+b.
Absorbance of each accessory dye reference blank extract calculated at 50mm optical path length; Absorbance of standard extract calculated at 10mm optical path length; Absorbance of standard reference blank extract calculated at 10mm optical path length; b
Converted into ratio calculated at 10mm optical path length; Reference concentration of standard extract based on 1% sample solution, %; S--total content of the sample.
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 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: 0.001 mg/mL. Take 1 mL of the standard solution containing 0.1 mg/mL arsenic (As) in a 100 mL volumetric flask and dilute to the scale.
4.7.2 Instruments and equipment
Apparatus according to the arsenic spot method in GB/T8450-1987. 4.7.3 Test method
Weigh 1.0 g of Amaranth 85 or Amaranth 60 sample, accurate to 0.01 g, and place in a round-bottom flask. Add 1.5 mL of nitric acid and 5 mL 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 5 mL of nitric acid-peroxy 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 5 mL 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 5 mL 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 and keep for 10 min. Let it cool and transfer it to a 100 mL 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 4479. 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 the sample of Broad Red 85 or Fluorescent Red 60, accurate to 0.01g, and place it in a crucible made of platinum (or quartz, porcelain), 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, and gradually heat it until sulfuric acid vapor almost stops. Put it in an electric furnace, burn it at 450C~550℃ until it is ash, and then cool it. Add 3mL of hydrochloric acid and shake it well, then add 7mL of water and shake it well, 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 liquid and the filtrate, and add water to make it 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 20 mL of the sample solution, put it into a Nessler colorimetric tube, add 1 drop of phenol test solution, add ammonia solution until the solution turns red, then add 2 mL of acetic acid solution, filter if necessary, wash the filter paper with water, and add water to make up to 50 mL 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 bath solution and 1 drop of phenol indicator solution, and 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 and stand 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 food additive Amaranth 85 or Amaranth 60 in accordance with the provisions of this standard. The production unit shall ensure that the quality of all food additives Amaranth 85 or Amaranth 60 shipped from the factory meets the requirements of this standard and has a quality certificate in a certain format.
5.2 Food additives Amaranth 85 or Amaranth 60 are a batch of homogenized products mixed once. 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 and dry ground-mouth glass bottles, seal them with paraffin, and label them with the manufacturer name, product name, batch number, and sampling date. One bottle is for inspection and the other bottle is kept for future reference. 5.4 If any index does not meet the requirements of this standard in the inspection results, samples should be taken from twice the amount of packaging for re-inspection. If the re-inspection results still do not meet the requirements of this standard, the batch of products will be unqualified. 5.5 The user has the right to accept the quality of the food additive Amaranth 85 or Amaranth 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 label name, shelf life, production date and batch number, net content, and instructions for use. 6.3 Food additives Amaranth 85 or Amaranth 60 are 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 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 meets the requirements of this standard. 349
A1 Reagents and materials
a) Hydrochloric acid:
b) Ammonium ferrous sulfate;
c) Ammonium thiocyanate solution: 200g/L
d) Sulfuric acid solution: 1+l;
GB 4479.1—1999
Appendix A
(Appendix to the standard)
Preparation method of titanium trifluoride standard titration solutione) Potassium dichromate standard titration solution: c(1/6KzCr20,)=0.1mol/L. A2 Instruments and equipment
See Figure 1.
A3 Preparation of titanium trichloride standard titration solution A3.1 Preparation
Put 100mL of titanium trichloride solution and 75mL of hydrochloric acid in a 1000mL brown volumetric flask, dilute to the mark with freshly boiled water that has been cooled to room temperature, shake well, and immediately pour into a light-proof bottle with a lower opening, 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 trinitride 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 according to formula (A1): V.xo
Wherein: Vi-
(A1)
Volume of potassium dichromate standard titration solution, mL: Volume of titanium trichloride standard titration solution consumed to titrate the oxidized high iron by potassium dichromate standard titration solution: mL; Volume of titanium trichloride standard titration solution consumed to titrate the blank, mL, Actual concentration of potassium dichromate standard titration solution, mol/L, Note: The above calibration needs to be performed immediately when analyzing the sample. 3501 Preparation
Take 100mL of titanium trichloride solution and 75mL of hydrochloric acid and place them in a 1000mL brown volumetric flask, dilute to the mark with water that has been freshly boiled and cooled to room temperature, shake well, and immediately pour into a light-proof lower-mouthed 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, and then titrate with the titanium trinitride 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. At the same time, a blank test should be performed in the same way by replacing potassium dichromate solution with 45mL of water.
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.xo
Wherein: Vi-
(A1)
The volume of potassium dichromate standard titration solution, mL: The volume of titanium trichloride standard titration solution consumed to titrate the oxidized high iron by potassium dichromate standard titration solution: mL; The volume of titanium trichloride standard titration solution consumed in the titration blank, mL, The actual concentration of potassium dichromate standard titration solution, mol/L, Note: The above calibration needs to be performed immediately when analyzing the sample. 3501 Preparation
Take 100mL of titanium trichloride solution and 75mL of hydrochloric acid and place them in a 1000mL brown volumetric flask, dilute to the mark with water that has been freshly boiled and cooled to room temperature, shake well, and immediately pour into a light-proof lower-mouthed 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, and then titrate with the titanium trinitride 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. At the same time, a blank test should be performed in the same way by replacing potassium dichromate solution with 45mL of water.
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.xo
Wherein: Vi-
(A1)
The volume of potassium dichromate standard titration solution, mL: The volume of titanium trichloride standard titration solution consumed to titrate the oxidized high iron by potassium dichromate standard titration solution: mL; The volume of titanium trichloride standard titration solution consumed in the titration blank, mL, The actual concentration of potassium dichromate standard titration solution, mol/L, Note: The above calibration needs to be performed immediately when analyzing the sample. 350
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