Some standard content:
GB 4479.2—1996
This standard is equivalent to the synthetic pigment lake test method and product standard part of the general test method in the sixth edition of the Japanese Food Additive Code.
The main differences between this standard and the Japanese standard are as follows: 1. The content index of this standard is ≥20.0%, while the index of Japan is ≥10.0%. 2. In addition to the titanium trichloride titration method, the spectrophotometry method is added to the product content determination in this standard. This method is used as the daily determination method. If there is a dispute between the supply and demand parties and arbitration is required, the titanium trichloride method is still used as the arbitration method. 3. The determination method of arsenic content in this standard basically adopts the general method of GB/T8450, with an index of ≤0.0003% (As), and the Japanese index is ≤0. 000 4% (As203).
4. The determination of secondary dye content in this standard adopts the method in WHO/FAO, with an index of ≤1.2%. This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Food Supervision and Inspection Institute of the Ministry of Health. The drafting units of this standard are Shanghai Dyestuff Research Institute and Shanghai Food Hygiene Supervision and Inspection Institute. The main drafters of this standard are Qiu Yumei, Liu Jing, Qian Kai, Shi Huaijiong and Yuan Yicheng. 351
1 Scope
National Standard of the People's Republic of China
Food additive
Amaranth aluminum lake
Food additive
Amaranth aluminum lake
GB 4479.21996
This standard specifies the requirements, test methods, inspection rules, marking and packaging of food additive amaranth aluminum lake. This standard is applicable to the pigment lake generated by the reaction of food additive amaranth and aluminum hydroxide. This product can be added to food as a colorant. Www.bzxZ.net
Molecular formula C2HN,OS
Relative molecular mass 538.54 (according to the 1991 international relative atomic mass) 2 Cited 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. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601—88 Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents GB/T602—88 Preparation of standard solution for determination of impurities of chemical reagents (negISO6353-1:82) GB/T603-88 Preparation of preparations and products used in test methods of chemical reagents (neqISO6353-1:82) GB/T6682—92 Specifications and test methods for laboratory water (evISO3696—87) GB/T8450-87 Determination method of impurities in food additives GB4479.1-1996 Food additive Amaranth 3 Requirements
3.1 Appearance: Rose red powder.
3.2 Food additive Amaranth red aluminum lake shall meet the requirements of Table 1: Table 1
Content (as color acid)
Loss on drying (135±2C)
Insoluble matter in hydrochloric acid and ammonia water
Water-soluble chloride (as NaCl) and sulfate (as NasSO,) Approved by the State Administration of Technical Supervision on September 13, 1996 352
Implementation on May 1, 1997
Subsidiary dye
Arsenic (As)
Heavy metal (as Pb)
Barium (Ba)
4 Test method
GB 4479.2-1996
Table 1 (end)
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) Hydrochloric acid;
b) Potassium dihydrogen phosphate: 13.6g/L solution; Preparation: Weigh 13.6g of potassium dihydrogen phosphate and dissolve it in water, dilute to 900ml, then use 70mL of 40g/L sodium hydroxide solution to adjust the solution to pH7, and dilute to the scale in a 1000mL volumetric flask. Ammonia water: (1+2) solution;
Hydrochloric acid: (1+3) solution;
Sodium hydroxide: 40g/I and 100g/L solution; e)
Amaranth red aluminum lake standard sample: content ≥20.0%. 4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Analysis steps
4.2.3.1 Weigh 0.5g sample, dissolve in 5mL concentrated hydrochloric acid, place in a 500mL volumetric flask, add potassium dihydrogen phosphate solution to the scale, shake well, then accurately pipette 2mL into a 50mL volumetric flask, and dilute to the scale with potassium dihydrogen phosphate solution. The maximum absorption wavelength of the solution should be 520±2nm.
4.2.3.2 Weigh 0.1g sample, add 5mL hydrochloric acid solution, and heat in a water bath for about 5min, shake to dissolve, the solution is clear and rose red, cool, neutralize with ammonia solution, the solution gradually becomes a rose red colloidal precipitate. 4.2.3.3 Weigh 0.1g sample, add 5mL 100g/L sodium hydroxide solution, heat in a water bath for 5min and shake to dissolve, the solution is clear and rose red, cool, neutralize with hydrochloric acid solution to neutrality, and form a rose red colloidal precipitate. 4.3 Determination of aluminum lake content in amaranth
4.3.1 Titanium trichloride titration method
4.3.1.1 Summary of method
In alkaline medium, the azo group in the dye is reduced and decomposed into amino compounds by titanium trichloride. The percentage of the dye is calculated based on the consumption of titanium trichloride standard titration solution.
4.3.1.2 Reagents and materials
a) Ammonium ferrous sulfate;
Hydrochloric acid;
Titanium nitride:
Trisodium citrate:
Ammonium thiocyanate: 200g/L solution;
Sulfuric acid: (1+9), (1+1) solution;
GB 4479.2—1996
Potassium dichromate: c(1/6K,Cr.0,)=0.1mol/L standard solution;g)
h) Titanium trichloride standard solution c(TiCl.)=0.1mol/L, the preparation method for new preparation shall be in accordance with Appendix A of GB4479.1—1996;i)
Carbon dioxide in cylinders.
4.3.1.3 Analysis steps
Weigh 7g of sample, accurate to 0.0002g, add 80mL of (1+9) sulfuric acid solution, and stir to dissolve at (40-50℃). Transfer to a 250ml volumetric flask, dilute to scale with freshly boiled water that has been cooled to room temperature, shake well, accurately pipette 50mL, place in a 500ml conical flask, add 30g of trisodium citrate and 200mL of water, assemble the instrument as shown in Figure (1) of GB4479.1-1996, heat to boiling while passing a stream of carbon dioxide gas below the liquid surface, and titrate with titanium trichloride standard titration solution until the end point is colorless. 4.3.1.4 Expression of analysis results
The mass percentage of amaranth aluminum lake (X,) is calculated according to formula (1): X = VX0/21511 × 100
m X 50/250
Wherein: V--the volume of titanium trichloride standard solution consumed in titrating the sample, mL; the actual concentration of titanium trichloride standard solution, mol/L: · (1)
0.1511--the mass of amaranth aluminum lake expressed in grams that is equivalent to 1.00mL titanium trichloride standard titration solution [cTiCi.) = 1.000mol/L] #
The mass of the sample, g.
4.3.1.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1%. The arithmetic mean shall be taken as the determination result. 4.3.2 Spectrophotometric colorimetric method
4.3.2.1 Method summary
After dissolving the sample and the standard sample with known content in water, measure their absorbance at the maximum absorption wavelength respectively, and then calculate the base content of the sample.
4.3.2.2 Reagents and materials
a) Sodium hydrogen tartrate;
b) Amaranth red aluminum lake standard sample: content ≥ 20.0%. 4.3.2.3 Instruments and equipment
Spectrophotometer, with 10mm colorimetric III.
4.3.2.4 Analysis steps
a) Preparation of amaranth red aluminum lake standard solution Weigh 0.5g of amaranth red aluminum lake standard, accurate to 0.0002g, add 20mL of water and about 2g of sodium hydrogen tartrate, slowly heat to 80~~~90C, transfer to a 500ml volumetric flask after dissolution, dilute to scale, shake well, accurately pipette 10mL and transfer to a 250mL volumetric flask, dilute to scale, shake well.
b) Preparation of Amaranth Aluminum Lake Sample Solution
Weighing and operation methods are the same as those for the preparation of standard solution. ) Operation
Measure the absorbance of the standard solution and the test solution at a wavelength of 520±2nm using a 10mm cuvette on a spectrophotometer. Use water as the reference solution.
4.3.2.5 Expression of analysis results
GB 4479.2—1996
The mass percentage of amaranth aluminum lake (X) is calculated according to formula (2): X,
Wherein: A. Absorbance of test solution:
A. Absorbance of standard solution;
X, mass percentage of amaranth aluminum lake standard sample (titanium chloride method). 4.3.2.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 2%, and the arithmetic mean shall be taken as the determination result. The above determination method uses titanium trifluoride titration as the arbitration method, and one of the determinations can be selected according to the conditions for daily inspection. 4.4 Determination of loss on drying
According to 4.4 of GB4479.1—1996.
4.5 Determination of insoluble matter content in hydrochloric acid and ammonia water 4.5.1 Reagents and materials
a) Hydrochloric acid:
b) Hydrochloric acid: (3+7) solution;
c) Ammonia water: (4+96) solution;
d) Silver nitrate: c(AgNO,)=0.1mol/L solution. 4.5.2 Analysis steps
Weigh 2g of sample, accurate to 0.01g, and place it in a 600mL beaker. Add 20mL of water and 20mL of concentrated hydrochloric acid. After fully stirring, add 300mL of hot water, stir well, cover with a watch glass, heat in a water bath at 70-80℃ for 30min, cool, and filter with a C4 sand core crucible that has been dried to constant weight at 135±2℃. Rinse the insoluble matter in the beaker into a jar with water until the washing liquid is colorless, then wash with 100mL of ammonia solution, wash with 10mL of hydrochloric acid solution, and then wash with water until the solution is free of white precipitate when detected by silver nitrate solution, and then place in a constant temperature oven at 135±2℃ and dry to constant weight.
4.5.3 Expression of analysis results
The mass percentage of insoluble matter in hydrochloric acid and ammonia water (X.) is calculated according to formula (3): X
Wherein: m2-
Mass of insoluble matter after drying,;
Mass of sample·.
m2×100
4.5.4 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.05%. The arithmetic mean shall be taken as the determination result. 4.6 Determination of the content of water-soluble chloride (in terms of NaCl) and sulfate (in terms of NazSO4) 4.6.1 Reagents and materials
a) Activated carbon;
Nitrobenzene;
Nitric acid: (1+1) solution;
Silver nitrate: c(AgNO4)=0.1mol/L standard solution; d)
·(3)
Ammonium thiocyanate: c(NH4CNS)=0.1mol/L standard solution; e)
Ammonium ferric sulfate solution: Weigh 14g of ammonium ferric sulfate, dissolve it in 100mL of water, filter, add 10mL of nitric acid, and store in a brown bottle. f)
4.6.2 Preparation of sample solution
Weigh 2 g of sample accurately to 0.001 g, add 200 mL of water accurately, stir evenly, let stand for 30 min (stir constantly during this period), filter with dry filter paper. If the filtrate is colored, add 2 g of activated carbon, stir occasionally and let stand for 1 h, then filter with dry filter paper. If there is still color, replace the activated carbon 355
and repeat the operation.
4.6.3 Determination of chloride (as NaCl) content 4.6.3.1 Analytical steps
GB 4479.2-1996
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 solution (add more when the chloride content is high) and 5mL of nitrobenzene. Shake vigorously until the silver chloride coagulates. Add 1mL of ammonium ferric sulfate test solution and titrate the excess silver nitrate to the end point with ammonium thiocyanate standard solution and keep it for 1min. At the same time, do a blank test in the same way. 4.6.3.2 Expression of analytical results
The mass percentage of chloride (X,) is calculated according to formula (4): (V/-V)XcX 0.058 4 × 100 = X
Wherein: V
m X 50/200
(V, - V) × c × 23.36
The volume of 0.1 mol/L ammonium thiocyanate standard solution used to titrate the sample, mL; V
-The volume of ammonium thiocyanate solution used to titrate the blank solution, mL: The concentration of the ammonium thiocyanate standard solution, mol/L:. (4)
The amount of chloride equivalent to 1.00 mL of ammonium thiocyanate standard titration solution [c(NH,CNS)=1.000mal/L], expressed in grams 0.058 4 -
Sodium mass:
Test mass, g.
4.6.3.3 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. 4.6.4 Determination of sulfate (in terms of NazSO.) content 4.6.4.1 Reagents and materials
a) Ammonia water,
Sodium hydroxide: 0.2g/L solution;
Hydrochloric acid: (1+99) solution;
Ethanol, 95%;
Tetrahydroxybenzoic acid disodium-potassium chloride: Mix equal amounts of mixed reagents; f)
Sulfuric acid: c(1/2H,SO)) =0.1mol/L standard solution; phenolphthalein: 10g/L ethanol solution;
h) Sodium rose bengalate indicator solution: weigh 0.1g sodium rose bengalate and dissolve it in 10mL water (prepare and use immediately); barium chloride: c(1/2BaCl2)=0.1mol/L standard solution; preparation: weigh 12.25g barium chloride, dissolve it in 500mL distilled water, transfer it into a 1000ml volumetric flask, dilute to the scale, and shake well. Calibration: absorb 20mL sulfuric acid standard solution, add 50mL water, and neutralize it 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 indication, and a rose red spot appears on the filter paper, which is maintained for 2min without fading as the end point. The concentration of the barium chloride standard solution (X2) is calculated according to formula (5): X2 =
Wherein: V—volume of sulfuric acid standard solution, mL; V2—volume of barium chloride standard solution, mL; concentration of sulfuric acid standard titration solution, mol/L. 4.6.4.2 Analysis steps
Pipette 25 mL of the test solution and place it in a 250 mL conical flask, add 1 drop of phenolic acid indicator, add sodium hydroxide solution until it turns pink, then add hydrochloric acid solution until the pink disappears, then add 30 mL of ethanol and 0.4 g+ of tetrahydroxybenzene disodium-potassium chloride mixed indicator and shake well. After dissolving, titrate with the 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 rose red sodium acid indicator solution as an external indicator. At the same time, perform a blank test in the same way. 356
4.6.4.3 Expression of analysis results
GB 4479.2-1996
The mass percentage of sodium sulfate (X.) shall be calculated according to formula (6): X
(V - V) X c X 0. 071 >
X 100
Wherein: V——-the volume of barium chloride standard solution consumed in titrating the sample solution, mL; V,——the volume of barium chloride standard solution consumed in titrating the blank solution, mL; (V - V) × c × 56. 8
the actual concentration of barium chloride standard solution, mol/L; 0.071——the mass of sodium sulfate equivalent to 1.00mL barium chloride standard titration solution [Lc (1/2BaCl2) = 1.000mol/L], expressed in grams·g;
the mass of the sample, g.
The sum of the mass percentage of chloride and sulfate, X, is calculated according to formula (7): X,X+X.
Where: X,--the mass percentage of chloride, %; X.--the mass percentage of sulfate, %; The sum of X+X. shall not be greater than 2.0%.
4.6.4.4 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 4.7 Determination of secondary dye content
4.7.1 Method Summary
Use paper chromatography to separate the components, elute, and then quantify by spectrophotometry. 4.7.2 Reagents and materials
According to 4.8.2 of GB4479.1-1996.
4.7.3 Instruments and equipment
According to 4.8.3 of GB4479.1-1996.
4.7.4 Analytical procedures
According to 4.8.4.1 of GB4479.1-1996. （
4.7.4.1 Preparation of sample eluate:
Weigh 2g of sample, accurate to 0.01g, place in a beaker, add 80mL of water and 5g of sodium hydrogen tartrate, slowly heat to 80-90°C, stir to dissolve, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Use a microinjector to accurately draw 100uL of the above 2% solution, evenly apply it on a baseline 25mm away from the bottom edge of the filter paper, in a straight line, so that its width on the filter paper does not exceed 5mm and its length is 130mm. Dry up with a hair dryer, filter paper is put into the chromatography cylinder and launched, the filter paper bottom is immersed in 10mm below the developer liquid level, treat that the developer front line rises to 150mm or until the secondary dye is separated satisfactorily, take out, dry up with cold wind with a hair dryer. Simultaneously launch under the same conditions with blank filter paper, the filter paper that this blank filter paper must be launched with the sample solution and is cut at adjacent positions on the filter paper of same (600mmX600mm). Chromatogram on secondary dye paper is pressed on chromatogram 2 on secondary dye paper among GB4479.1-199. Each secondary dye and in the air Cut the filter paper corresponding to each secondary dye on the white filter paper into the same size and place them in 50mL Nessler colorimetric tubes. Add 5mL of acetone solution accurately to each tube. After shaking for 3-5 minutes, add 20mL of sodium bicarbonate solution accurately and shake thoroughly. Filter the extracts naturally in No. 3 glass sand core funnels. Pour the filtrate into a 50mm thick colorimetric tube and measure the absorbance at the maximum absorption wavelength of each secondary dye with a spectrophotometer. Use a mixture of 5mL of acetone solution and 20mL of sodium bicarbonate solution as the reference solution. 4. 7.4.2 Preparation of standard eluate
Accurately pipette 6 ml of the above 2% sample solution. Transfer to a 100 mL volumetric flask, dilute to the mark, and shake well. Use a microinjector to pipette 100 μl and evenly apply it on a baseline 25 mm from the bottom edge of the filter paper. When the front line of the developing agent rises only 40 mm, take it out and blow it dry. Cut off all the dye parts developed under 357
GB4479.2-1996
, perform the extraction operation as before, and measure the absorbance at the maximum absorption wavelength with a 10 mm cuvette. At the same time, use a blank filter paper to develop under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.4.3 Expression of analysis results
The mass percentage of the secondary dye (X.) is calculated according to formula (8): X - [(A-6)++(A-6)]/5)
(A, —b,)
Wherein: A, A.-the absorbance of each secondary dye extract calculated at a light path length of 50 mm; b, **, bn
the absorbance of each secondary dye reference blank extract calculated at a light path length of 50 mm; A.-the absorbance of the standard extract calculated at a light path length of 10 mm; b. the absorbance of the standard reference blank sample calculated at a light path length of 10 mm; 5-the ratio converted to a light path length of 10 mm;
6-the reference concentration of the standard extract based on the 2% sample solution, %; S---the total content of the sample, %.
4.7.4.4 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. 4.8 Determination of arsenic content
According to 4.9 of GB4479.1-1996.
4.9 Determination of heavy metal content
4.9.1 Summary of method
(8)
The sample shall be carbonized and ashed at high temperature, cooled, dissolved and filtered with acid, diluted to a certain volume, and sodium sulfide shall be added when the pH is equal to 4, and then limited colorimetry shall be performed.
4.9.2 Reagents and materials
Sulfuric acid;
Hydrochloric acid;
Nitric acid;
Hydrochloric acid: (1+3) solution;
Ammonium acetate: (1+9) solution:
Sodium sulfide: 100g/L solution;
Lead standard push solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2g of the sample, accurate to 0.01g, put it in a porcelain, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace and burn it at 450-550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, grind it thoroughly, and evaporate it to dryness on a water bath. Add 5mL of hydrochloric acid, crush the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washings, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washings, adjust with ammonium acetate solution to H = 4, add water to 100mL, as the sample solution. Perform the same operation as a blank test. Take 40mL of the sample solution, add water to 50mL, as the detection solution. Take 40mL of the blank test solution, add 2ml of the lead standard solution: add water to 50mL, as the comparison solution.
4.10 Determination of iodine content
4.10.1 Reagents and materials
a) Sulfuric acid;
Sulfuric acid: 1+19) solution
c) Hydrochloric acid (1+3) solution.
4.10.2 Analysis steps
GB4479.21996
Accurately weigh 1g of the sample, accurate to 0.01, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, slowly heat it, and try to make it almost completely ash at a low temperature: let it cool, add 1mL of sulfuric acid, slowly heat it until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450-550 for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix it thoroughly, cover it and heat it to melt. Continue heating for 10min, cool it, add 20ml of water and heat it in a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not show sulfate reaction. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10ml of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix, and leave it for 10 minutes, and it should not be turbid.
5 Inspection rules
5.1 In the quality inspection of food additive amaranth aluminum lake, the determination of barium content is a type inspection, which is sampled once every quarter, and the other 7 items are! "inspection.
5.2 Except for each large box of 10X200g, the rest are in accordance with Chapter 5 of GB4479.1-1996. 6 Marking and packaging
6.1 Except for each small package of 200g, the rest are in accordance with Chapter 6 of GB4479.1-1996. 3591-199, the side dye on paper chromatogram 2. Cut each side dye and the filter paper corresponding to each side dye on the blank filter paper into the same size, place them in 50mL Nessler colorimetric tubes, accurately add 5mL of acetone solution to each, shake for 3~5min, then accurately add 20mL of sodium bicarbonate solution, shake thoroughly, filter the extracts naturally in No. 3 glass sand core funnels, pour the filtrate into a 50mm thick colorimetric blood, and use a spectrophotometer to measure the absorbance at the maximum absorption wavelength of each side dye. Use a mixture of 5ml of acetone solution and 20mL of sodium bicarbonate solution as the reference solution. 4.7.4.2 Preparation of standard eluate
Accurately pipette 6ml of the above 2% sample solution. Transfer it to a 100mL volumetric flask, dilute to the mark, and shake well. Use a micro-injector to absorb 100) μl and evenly apply it on a baseline 25 mm from the bottom edge of the filter paper. When the front line of the developing agent rises only 40 mm, take it out and blow it dry. Cut all the dye parts developed under 357
GB4479.2-1996
, and perform the extraction operation as before. Use a 10 mm cuvette to measure the absorbance at the maximum absorption wavelength. At the same time, use a blank filter paper to develop under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.4.3 Expression of analysis results
The mass percentage of the secondary dye (X.) is calculated according to formula (8): X - [(A-6)++(A-6)]/5)
(A, —b,)
Wherein: A, A.-the absorbance of each secondary dye extract calculated at a light path length of 50 mm; b, **, bn
the absorbance of each secondary dye reference blank extract calculated at a light path length of 50 mm; A.-the absorbance of the standard extract calculated at a light path length of 10 mm; b. the absorbance of the standard reference blank sample calculated at a light path length of 10 mm; 5-the ratio converted to a light path length of 10 mm;
6-the reference concentration of the standard extract based on the 2% sample solution, %; S---the total content of the sample, %.
4.7.4.4 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. 4.8 Determination of arsenic content
According to 4.9 of GB4479.1-1996.
4.9 Determination of heavy metal content
4.9.1 Summary of method
(8)
The sample shall be carbonized and ashed at high temperature, cooled, dissolved and filtered with acid, diluted to a certain volume, and sodium sulfide shall be added when the pH is equal to 4, and then limited colorimetry shall be performed.
4.9.2 Reagents and materials
Sulfuric acid;
Hydrochloric acid;
Nitric acid;
Hydrochloric acid: (1+3) solution;
Ammonium acetate: (1+9) solution:
Sodium sulfide: 100g/L solution;
Lead standard push solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2g of the sample, accurate to 0.01g, put it in a porcelain, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace and burn it at 450-550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, grind it thoroughly, and evaporate it to dryness on a water bath. Add 5mL of hydrochloric acid, crush the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washings, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washings, adjust with ammonium acetate solution to H = 4, add water to 100mL, as the sample solution. Perform the same operation as a blank test. Take 40mL of the sample solution, add water to 50mL, as the detection solution. Take 40mL of the blank test solution, add 2ml of the lead standard solution: add water to 50mL, as the comparison solution.
4.10 Determination of iodine content
4.10.1 Reagents and materials
a) Sulfuric acid;
Sulfuric acid: 1+19) solution
c) Hydrochloric acid (1+3) solution.
4.10.2 Analysis steps
GB4479.21996
Accurately weigh 1g of the sample, accurate to 0.01, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, slowly heat it, and try to make it almost completely ash at a low temperature: let it cool, add 1mL of sulfuric acid, slowly heat it until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450-550 for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix it thoroughly, cover it and heat it to melt. Continue heating for 10min, cool it, add 20ml of water and heat it in a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not show sulfate reaction. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10ml of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix, and leave it for 10 minutes, and it should not be turbid.
5 Inspection rules
5.1 In the quality inspection of food additive amaranth aluminum lake, the determination of barium content is a type inspection, which is sampled once every quarter, and the other 7 items are! "inspection.
5.2 Except for each large box of 10X200g, the rest are in accordance with Chapter 5 of GB4479.1-1996. 6 Marking and packaging
6.1 Except for each small package of 200g, the rest are in accordance with Chapter 6 of GB4479.1-1996. 3591-199, the side dye on paper chromatogram 2. Cut each side dye and the filter paper corresponding to each side dye on the blank filter paper into the same size, place them in 50mL Nessler colorimetric tubes, accurately add 5mL of acetone solution to each, shake for 3~5min, then accurately add 20mL of sodium bicarbonate solution, shake thoroughly, filter the extracts naturally in No. 3 glass sand core funnels, pour the filtrate into a 50mm thick colorimetric blood, and use a spectrophotometer to measure the absorbance at the maximum absorption wavelength of each side dye. Use a mixture of 5ml of acetone solution and 20mL of sodium bicarbonate solution as the reference solution. 4.7.4.2 Preparation of standard eluate
Accurately pipette 6ml of the above 2% sample solution. Transfer it to a 100mL volumetric flask, dilute to the mark, and shake well. Use a micro-injector to absorb 100) μl and evenly apply it on a baseline 25 mm from the bottom edge of the filter paper. When the front line of the developing agent rises only 40 mm, take it out and blow it dry. Cut all the dye parts developed under 357
GB4479.2-1996
, and perform the extraction operation as before. Use a 10 mm cuvette to measure the absorbance at the maximum absorption wavelength. At the same time, use a blank filter paper to develop under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.4.3 Expression of analysis results
The mass percentage of the secondary dye (X.) is calculated according to formula (8): X - [(A-6)++(A-6)]/5)
(A, —b,)
Wherein: A, A.-the absorbance of each secondary dye extract calculated at a light path length of 50 mm; b, **, bn
the absorbance of each secondary dye reference blank extract calculated at a light path length of 50 mm; A.-the absorbance of the standard extract calculated at a light path length of 10 mm; b. the absorbance of the standard reference blank sample calculated at a light path length of 10 mm; 5-the ratio converted to a light path length of 10 mm;
6-the reference concentration of the standard extract based on the 2% sample solution, %; S---the total content of the sample, %.
4.7.4.4 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. 4.8 Determination of arsenic content
According to 4.9 of GB4479.1-1996.
4.9 Determination of heavy metal content
4.9.1 Summary of method
(8)
The sample shall be carbonized and ashed at high temperature, cooled, dissolved and filtered with acid, diluted to a certain volume, and sodium sulfide shall be added when the pH is equal to 4, and then limited colorimetry shall be performed.
4.9.2 Reagents and materials
Sulfuric acid;
Hydrochloric acid;
Nitric acid;
Hydrochloric acid: (1+3) solution;
Ammonium acetate: (1+9) solution:
Sodium sulfide: 100g/L solution;
Lead standard push solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2g of the sample, accurate to 0.01g, put it in a porcelain, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace and burn it at 450-550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, grind it thoroughly, and evaporate it to dryness on a water bath. Add 5mL of hydrochloric acid, crush the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washings, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washings, adjust with ammonium acetate solution to H = 4, add water to 100mL, as the sample solution. Perform the same operation as a blank test. Take 40mL of the sample solution, add water to 50mL, as the detection solution. Take 40mL of the blank test solution, add 2ml of the lead standard solution: add water to 50mL, as the comparison solution.
4.10 Determination of iodine content
4.10.1 Reagents and materials
a) Sulfuric acid;
Sulfuric acid: 1+19) solution
c) Hydrochloric acid (1+3) solution.
4.10.2 Analysis steps
GB4479.21996
Accurately weigh 1g of the sample, accurate to 0.01, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, slowly heat it, and try to make it almost completely ash at a low temperature: let it cool, add 1mL of sulfuric acid, slowly heat it until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450-550 for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix it thoroughly, cover it and heat it to melt. Continue heating for 10min, cool it, add 20ml of water and heat it in a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not show sulfate reaction. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10ml of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix, and leave it for 10 minutes, and it should not be turbid.
5 Inspection rules
5.1 In the quality inspection of food additive amaranth aluminum lake, the determination of barium content is a type inspection, which is sampled once every quarter, and the other 7 items are! "inspection.
5.2 Except for each large box of 10X200g, the rest are in accordance with Chapter 5 of GB4479.1-1996. 6 Marking and packaging
6.1 Except for each small package of 200g, the rest are in accordance with Chapter 6 of GB4479.1-1996. 3592 Reagents and materials
Sulfuric acid;
Hydrochloric acid;
Nitric acid;
Hydrochloric acid: (1+3) solution;
Ammonium acetate: (1+9) solution;
Sodium sulfide: 100g/L solution;
Lead standard push solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2g of the sample, accurate to 0.01g, put it in a porcelain, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace and burn it at 450-550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, grind it thoroughly, and evaporate it to dryness on a water bath. Add 5mL of hydrochloric acid, crush the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washings, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washings, adjust with ammonium acetate solution to H = 4, add water to 100mL, as the sample solution. Perform the same operation as a blank test. Take 40mL of the sample solution, add water to 50mL, as the detection solution. Take 40mL of the blank test solution, add 2ml of the lead standard solution: add water to 50mL, as the comparison solution.
4.10 Determination of iodine content
4.10.1 Reagents and materials
a) Sulfuric acid;
Sulfuric acid: 1+19) solution
c) Hydrochloric acid (1+3) solution.
4.10.2 Analysis steps
GB4479.21996
Accurately weigh 1g of the sample, accurate to 0.01, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, slowly heat it, and try to make it almost completely ash at a low temperature: let it cool, add 1mL of sulfuric acid, slowly heat it until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450-550 for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix it thoroughly, cover it and heat it to melt. Continue heating for 10min, cool it, add 20ml of water and heat it in a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not show sulfate reaction. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10ml of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix, and leave it for 10 minutes, and it should not be turbid.
5 Inspection rules
5.1 In the quality inspection of food additive amaranth aluminum lake, the determination of barium content is a type inspection, which is sampled once every quarter, and the other 7 items are! "inspection.
5.2 Except for each large box of 10X200g, the rest are in accordance with Chapter 5 of GB4479.1-1996. 6 Marking and packaging
6.1 Except for each small package of 200g, the rest are in accordance with Chapter 6 of GB4479.1-1996. 3592 Reagents and materials
Sulfuric acid;
Hydrochloric acid;
Nitric acid;
Hydrochloric acid: (1+3) solution;
Ammonium acetate: (1+9) solution;
Sodium sulfide: 100g/L solution;
Lead standard push solution: dilute 10 times when used, 1mL contains 0.01mg lead. 4.9.3 Analysis steps
Weigh 2g of the sample, accurate to 0.01g, put it in a porcelain, add a little sulfuric acid to moisten it, slowly burn it, try to ash it at low temperature, cool it, add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops, put it in an electric furnace and burn it at 450-550℃ for 3h, then cool it. Add 5mL of hydrochloric acid and 1mL of nitric acid, grind it thoroughly, and evaporate it to dryness on a water bath. Add 5mL of hydrochloric acid, crush the block thoroughly, heat to dissolve, evaporate to dryness on a water bath. Add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter with quantitative analysis filter paper (No. 5C), wash the residue with about 30mL of hydrochloric acid solution, combine the filtrate and washings, evaporate to dryness on a water bath, add 10mL of hydrochloric acid solution, heat to dissolve, cool, filter, wash with a small amount of water, combine the filtrate and washings, adjust with ammonium acetate solution to H = 4, add water to 100mL, as the sample solution. Perform the same operation as a blank test. Take 40mL of the sample solution, add water to 50mL, as the detection solution. Take 40mL of the blank test solution, add 2ml of the lead standard solution: add water to 50mL, as the comparison solution.
4.10 Determination of iodine content
4.10.1 Reagents and materials
a) Sulfuric acid;
Sulfuric acid: 1+19) solution
c) Hydrochloric acid (1+3) solution.
4.10.2 Analysis steps
GB4479.21996
Accurately weigh 1g of the sample, accurate to 0.01, put it in a platinum crucible, add a small amount of sulfuric acid to moisten it, slowly heat it, and try to make it almost completely ash at a low temperature: let it cool, add 1mL of sulfuric acid, slowly heat it until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450-550 for 3h. After cooling, add 5g of anhydrous sodium carbonate and mix it thoroughly, cover it and heat it to melt. Continue heating for 10min, cool it, add 20ml of water and heat it in a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not show sulfate reaction. Then move the residue on the paper and the filter paper into a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10ml of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix, and leave it for 10 minutes, and it should not be turbid.
5 Inspection rules
5.1 In the quality inspection of food additive amaranth aluminum lake, the determination of barium content is a type inspection, which is sampled once every quarter, and the other 7 items are! "inspection.
5.2 Except for each large box of 10X200g, the rest are in accordance with Chapter 5 of GB4479.1-1996. 6 Marking and packaging
6.1 Except for each small package of 200g, the rest are in accordance with Chapter 6 of GB4479.1-1996.359
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