Some standard content:
GB 4480.1—2001
All technical contents of this standard are mandatory. Former
This standard is equivalent to the sixth edition (1992) of the "Japanese Food Additives Code" "Edible Red No. 102 (Carmine)", which is a revision of GB4480.1—1994 "Food Additive Carmine". The main technical differences between this standard and the Japanese standard are: 1. The heavy metal (in terms of Pb) index in this standard is ≤0.001%, and the Japanese index is ≤0.002%. 2. The determination of arsenic content in this standard continues to use GB/T8450-1987 "Determination Method of Pb in Food Additives", and the index is ≤0.000 1% (in terms of As), and the Japanese index is ≤0.000 4% (As2O3). 3. The determination of secondary dye content in this standard continues to use the determination method in GB4480.1-1994, and the index is ≤3.0%. 4. In addition to the titanium trifluoride titration method, this standard adds a relatively simple spectrophotometric method for daily determination. The titanium trichloride method is used as the arbitration method.
5. The determination method of chloride (in terms of NaC1) and sulfate (in terms of NazSO.) in this standard is chemical titration, while the Japanese standard is ion chromatography.
The main technical differences between this standard and GB4480.1-1994 are as follows: 1. GB4480.1-1994 has two specifications of Carmine 82 and Carmine 60, and this standard cancels the Carmine 60 specification. Since the fact that the structure of carmine contains 1.5% of crystal water has been confirmed in the sixth edition of the "Japanese Food Additives Official Book", the corresponding amount has been modified and its content has been changed to ≥85.0%. Therefore, the content of this standard has also been revised to ≥85.0%. 2. This standard adds the determination items of chloride (in terms of NaCl) and sulfate (in terms of Na?SO), with an index of ≤8.0%. 3. The determination item of isopropyl ether extract content has been cancelled. This standard will replace GB4480.1-1994 from the date of implementation. Appendix A in this standard is the appendix of the standard.|| tt||This standard is proposed by the State Bureau 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. The drafting units of this standard are: Shanghai Dye Research Institute and Shanghai Municipal Health Bureau Health Supervision Institute. The main drafters of this standard are: Ding Deyi, Liu Jing, Li Yuhua, Shi Huaijiong, Zhou Yanqin. This standard is entrusted to the Chemical Branch of the National Technical Committee on Food Additive Standardization for interpretation. This standard was first issued in 1988 and revised for the first time in 1994. 360
National Standard of the People's Republic of China
Food Additives
Cholesteatin
Food additive--Ponceau 4R
GB 4480. 1---2001
Replaces GB4480.1-·1994
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of the food additive carmine. This standard is applicable to food, cosmetics and other industries as a colorant. Structural formula:
Molecular formula: C2HuN2NaOS3·1.5H
Relative molecular mass: 631.51 (according to the 1997 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T 601—19881
Preparation of standard solutions for determination of impurities in chemical reagents GB/T602—19881
Preparation of preparations and products used in test methods for chemical reagents GB/T 603-—19881
Specifications and test methods for water used in analytical laboratories (neqISO3696:1987) GB/T 6682--1992
GB/T 8450--1987
3 Requirements
3.1 Appearance
Determination of arsenic in food additives
This product is red to dark red powder or granules. 3.2 Quality requirements
Should meet the requirements of Table 1.
Loss on drying
Total amount of chloride (calculated as NaCl) and sulfate (calculated as NazSO.) Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on October 24, 2001
Implementation on June 1, 2002
4 Test methods
Water-insoluble matter
Subsidiary dyes
Arsenic (calculated as As)
Heavy metals (calculated as Pb)
GB 4480.1-2001
Table 1 (End)
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T6682. Standard solutions, impurity standard solutions, preparations and products required in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
4.1 Appearance
Visually measure under natural light conditions, and the results shall comply with the provisions of 3.1 of this standard. 4.2 Identification
4.2.1 Reagents and materials
4.2.1.1 Sulfuric acid solution: 1-100.
4.2.1.2 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 to form a red clear solution. 4.2.3.2 Take 40mL of the red clear solution in 4.2.3.1 and add 10mL of sulfuric acid solution. The solution is purple-red. Take 2-3 drops of this solution and add it to 5mL of water to form a red solution with yellow light. 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 100mL. The maximum absorption wavelength of the solution is (508±2)nm. 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) Trisodium citrate;
b) Titanium trichloride standard titration solution: c (TiCl:) = 0.1 mol/L (newly prepared, ready for use, preparation method see Appendix A): ℃) Carbon dioxide in a cylinder.
4.3.1.3 Analysis steps
Weigh 5 samples, accurate to 0.0002g. Dissolve in 100 mL of water that has been freshly boiled and cooled to room temperature, transfer to a 500 mL volumetric flask, dilute to the mark, shake well, pipette 50 mL, place in a 500 mL conical flask, add 15 g of trisodium citrate and 150 mL of water, assemble the apparatus 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 colorless.
GB 4480.1—2001
1-conical flask (500mL); 2-brown burette (50mL); 3-bottomed glass bottle wrapped with black paper (2000mL); 4-container for a mixture of 10% ammonium carbonate and 10% ferrous sulfate in equal amounts (5000mL) 15-piston; 6-empty bottle; 7-gas washing bottle filled with water
Figure 1 Apparatus diagram for titanium trichloride titration
4.3.1.4 Expression of analytical results
Express the content of cerebral lipid red (X,) in mass percentage and calculate according to formula (1): X, = VXc×0.1579 ×100
VX cX 157.9
Where: V—-volume of titanium trichloride standard titration solution consumed for titration of sample, mL; c---actual concentration of titanium trichloride standard titration solution, mol/L; mass of sample, g;
0.1579——mass of carmine in grams equivalent to 1.00mL titanium trichloride standard titration solution [c(TiCls)=1.000mol/L].
4.3.1.5 Allowable difference
The difference between the results of the two determinations of the same sample shall not exceed 1.0%, and the arithmetic mean shall be taken as the determination result. 4.3.2 Spectrophotometric colorimetry
4.3.2.1 Method Summary
After dissolving the sample and the standard sample with known content in water, measure their absorbance at the maximum absorption wavelength, and then calculate the content of the sample.
4.3.2.2 Reagents and Materials
Carmine standard sample: ≥85.0% self-made, content determined by titanium trichloride titration. 4.3.2.3 Instruments and Equipment
a) Spectrophotometer;
b) Cuvette: 10 mm.
4.3.2.4 Preparation of Carmine Standard Solution
Weigh 0.5g of Carmine standard sample, accurate to 0.0002g. Dissolve in appropriate amount of water, transfer to a 1000ml volumetric flask, dilute to scale, and shake well. Pipette 10ml, transfer to a 500ml volumetric flask, dilute to scale, and shake well. 363
4.3.2.5 Preparation of carmine test solution
GB 4480.1-2001
Weigh 0.5g of the sample, and the rest is the same as the preparation of the standard solution. 4.3.2.6 Analysis steps
Place the standard solution and the sample solution in 10mm colorimetric blood, and measure the absorbance of each at a wavelength of (508±2)nm using a spectrophotometer,
using water as the reference solution.
4.3.2.7 Expression of analysis results
Express the carmine content (X,) in mass percentage, and calculate according to formula (2): AX×100
Absorbance of the sample solution;
Where: 4
Absorbance of the standard solution;
Mass percentage of the carmine 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%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of loss on drying
4.4.1 Analysis steps
(2)
Weigh 2g of the sample to the nearest 0.01g. Place it in a (30~~40)mm weighing bottle that has been constant weight, and dry it in a (135±2)℃ constant temperature oven to constant weight.
4.4.2 Expression of analysis results Www.bzxZ.net
Express the content (X) of loss on drying as mass percentage, calculated according to formula (3): m2-m ×100
Where: m2\--mass of the sample before drying g mass of the sample after drying to constant weight·g.
4.4.3 Allowable error
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. 4.5 Determination of chloride (as NaCI) and sulfate (as Na.SO.) content 4.5.1 Determination of chloride (as NaCI) content 4.5.1.1 Reagents and materials
a) Activated carbon:
h) Nitrobenzene;
c) Nitric acid solution: 1+1;
d) Silver nitrate solution: c(AgNO,)=0.1mol/L: e) Ammonium thiocyanate standard titration solution: c(NH,CNS)=0.1mol/Lf) 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 it in a brown bottle. ..(3)
4.5.1.2 Preparation of test solution
Weigh about 2g of carmine sample, accurate to 0.001g. Place in a 200mL volumetric flask and add appropriate amount of water. Add 10g of activated carbon and then 1ml of nitric acid solution. Add water to the scale, shake evenly, leave for 30min (shake occasionally during this period), filter with dry filter paper, if the filtrate is colored, use instructions:
1 Door H This standard adopts ion chromatography, this standard adopts chemical titration. 361
GB 4480. 1-2001
then add 2g of activated carbon, leave for 1h with occasional shaking, and filter with dry filter paper. If there is still color, replace the activated carbon and repeat the operation. 4.5.1.3 Analysis steps
Pipette 50ml of the test solution in 4.5.1.2 into a 500ml conical flask, add 2ml of nitric acid solution and 10ml of silver nitrate 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. Perform a blank test at the same time. 4.5.1.4 Expression of analytical results
Express the chloride content (in terms of NaCl) (X) in mass percentage and calculate it according to formula (4): X = (V) × cX 0.0584 × 100 = (V, V) X c × 23.36
m×200
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·mol/L; ...*.(4)
m—mass of sample, g;
0.0584—the mass of sodium chloride in grams equivalent to 1.00 mL of ammonium thiocyanate standard titration solution [c(NH,CNS)=1.000mol/L].
4.5.1.5 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. 4.5.2 Determination of sulfate (in terms of NazSO,) 4.5.2.1 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: mix in equal amounts;f) Standard sulfuric acid titration solution: c(1/2H,SO,)=0.1mol/L;g) Phenolphthalein indicator solution: 10g/L;
h) Sodium rhodamine indicator solution: weigh 0.1g sodium rhodamine and dissolve it in 10mL water (prepared and used immediately). i) Barium chloride standard titration solution: c(1/2BaCl.)=0.1mol/L. Preparation: Weigh 12.25g of barium chloride, dissolve in 500mL of water, transfer to a 1000mL volumetric flask, dilute to the mark, and shake to hook. Calibration: Take 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 rose red sodium indicator solution as an external indicator, and the end point is when a rose red spot appears on the filter paper and does not fade for 2 minutes. The concentration of the barium chloride standard titration solution (X,) is calculated according to formula (5): Vc
volume of sulfuric acid standard titration solution, mL;
wherein: V——
volume of barium chloride standard titration solution, mL
actual concentration of sulfuric acid standard titration solution, mol /I.(5)
4.5.2.2 Analysis steps
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 disappears, then add 30mL of ethanol and 0.4g of tetrahydroxybenzoic acid disodium-potassium chloride mixed indicator and shake well, dissolve and titrate with barium chloride standard solution under continuous shaking, use rose red sodium indicator solution as external indicator, and the end point is a rose red spot on the filter paper that does not fade for 2 minutes. Perform a blank test at the same time. 365
4.5.2.3 Expression of analysis results
GB 4480.1-2001
Express the sulfate content (in terms of Na2SO4) in mass percentage (X) and calculate it according to formula (6): X = (V- Vi) × c × 0.071 *
X 100 =
(V - Vi) X c X 56. 8
Wherein: V is the volume of barium chloride standard titration solution consumed in titrating the sample solution, mL; V is the volume of barium chloride standard titration solution consumed in titrating the blank solution, mL; c is the actual concentration of barium chloride standard titration solution, mol/L m is the mass of the sample, g;
0.071----the mass of sodium sulfate in grams equivalent to 1.00mL barium chloride standard titration solution [c (1/2BaC1,) = 1.000mol/L], g.
4.5.2.4 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. 4.5.3 Expression of analysis results
The sum of the contents of chloride (in terms of NaCl) and sulfate (in terms of Na2SO4) (X,) expressed in mass percentage is calculated according to formula (7): X, -X+X
Wherein: X, — the content of chloride expressed in mass percentage, %; X. — the content of sulfate expressed in mass percentage, %. The sum of X. + X. shall not be greater than 5.0%.
4.6 Determination of water-insoluble matter content
4.6.1 Analysis steps
Weigh about 3g of the sample, accurate to 0.01g. Place in a 500mL beaker, add 250mL of 50~60℃ water to dissolve it, filter it with 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 (135±2)℃ constant temperature oven to constant weight.
4.6.2 Expression of analysis results
Express the content of water-insoluble matter (X.) as mass percentage, calculated according to formula (8): ml×100
Where; m1——the mass of water-insoluble matter after drying, g: the mass of a sample, g.
4.6.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.10%, and the arithmetic mean shall be taken as the determination result. 4.7 Determination of secondary dye content 1
4.7.1 Method summary
Use paper chromatography to separate and elute the components, and then use spectrophotometry to quantify. 4.7.2 Reagents and materials
4.7.2.1 Anhydrous ethanol.
4.7.2.2 n-Butanol.
4.7.2.3 Acetone solution: 1+1.
4.7.2.4 Ammonia solution: 4+96.
4.7.2.5 Sodium bicarbonate solution: 4g/L.
4.7.3 Instruments and equipment
Instructions for use:
1 The Japanese standard uses the spot method, and this standard uses the original GB4480.1-1994 method to determine the content of secondary dyes. 366
4.7.3.1 Spectrophotometer.
GB4480.1-2001
4.7.3.2 Chromatographic filter paper: No. 1 medium speed, 150mm×250mm. 4.7.3.3 Chromatographic cylinder: 240mm×300mm. 4.7.3.4 Micro-injector: 100μl.
4.7.4 Analysis steps
4.7.4.1 Paper chromatography conditions
Developing solvent: n-butanol + anhydrous ethanol + ammonia solution = 6+2+3; temperature 20~25°C.
4.7.4.2 Preparation of sample eluate
Weigh 1g of carmine sample, accurate to 0.01g. Place in a beaker, add appropriate amount of water to dissolve, transfer to a 100mL volumetric flask, dilute to scale, shake, draw 100μL with a microinjector, evenly apply on a baseline 25mm away from the bottom edge of the filter paper, forming 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 into the chromatography cylinder saturated with solvent to develop, and immerse the bottom edge of the filter paper 10mm below the liquid surface of the developer. When the front line of the developer rises to 150mm or until the secondary dye is separated satisfactorily, take out the chromatography filter paper and blow dry with a hair dryer with cold air. At the same time, use blank filter paper to develop 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
Xie dye (1)
Secondary dye (2)
Main dye
Alcohol dye (3)
Secondary dye (4)
Figure 2 Schematic diagram of secondary dye chromatography
Cut each secondary dye and the filter paper corresponding to each secondary dye on the blank filter paper into the same size, and cut into thin strips of about 5mm×15mm, respectively placed in 50mL Nessler colorimetric tubes, accurately add 5mL of acetone solution, shake for 3~5min, then accurately add 20mL of sodium bicarbonate solution, shake thoroughly, and filter the extracts naturally in No. 3 glass sand core funnels. The filtrate must be clear and free of suspended matter. At the maximum absorption wavelength of each secondary dye, use a 50mm colorimetric dish to measure the absorbance on a spectrophotometer. Use a mixture of 5mL acetone solution and 20mL sodium bicarbonate solution as the reference solution. 4.7.4.3 Preparation of standard sample eluate
Accurately pipette 2 mL of the above 1% test solution into a 100 mL volumetric flask, dilute to the mark, and shake well. Use a microinjector to pipette 100 mL and evenly apply a dot on a baseline 25 mm from the bottom edge of the filter paper. Blow it with cold air. Place the filter paper in a solvent-saturated chromatography cylinder and develop it. Wait until the front line of the developing agent rises 40 mm. Take it out and blow it dry. Cut off all the dye parts. Perform the extraction operation as before. Use a 10 mm thick cuvette to measure the absorbance at the maximum absorption wavelength. 367
GB 4480. 1-2001
At the same time, develop it with a blank filter paper under the same conditions. After the same operation, measure the absorbance of the extract. 4.7.4.4 Expression of analytical results
Express the content of the secondary dye (X) in mass percentage. Calculate X according to formula (9): = E(A- - b) + +-. +(A. - 6.)]/5A6
Wherein.A,...A.
The absorbance of each secondary dye extract calculated at 50mm optical path length; the absorbance of each secondary dye control blank extract calculated at 50mm optical path length; the absorbance of the standard extract calculated at 10mm optical path length; the absorbance of the standard control blank extract calculated at 10 mm optical path length. Converted into a ratio calculated at 10mm optical path length; 2
The reference concentration of the standard extract based on 1% test solution, %; S total content of the sample.
4.7.4.5 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. 4.8 Determination of Arsenic Content
4.8.1 Reagents and Materials
4.8.1.1 Nitric Acid;
4.8.1.2 Sulfuric Acid Solution: 1+1.
4.8.1.3 Nitric Acid-Perchloric Acid Mixture: 3-1. (9)
4.8.1.4 Arsenic Standard Solution (0.001 mg/ml): Take 1 mL of 0.1 mg/ml standard solution in a 100 mL volumetric flask and dilute to the mark.
4.8.2 Instruments and Equipment
According to the Arsenic Spot Method Apparatus in GB/T8450-1987. 4.8.3 Analysis Procedure
Weigh 1.0 g of carmine sample to an accuracy of 0.01 g. Place in a round-bottom flask, add 1.5mL nitric acid and 5mL sulfuric acid solution, heat with low heat to drive out nitrogen dioxide gas, stop heating when the solution turns brown, cool and add 5mL nitric acid-perchloric acid mixture, heat with strong heat until the solution is transparent and colorless or slightly yellow. If it is still opaque, cool and add 5mL nitric acid-perchloric acid mixture, continue heating until the solution is clear and colorless or slightly yellow and produces white smoke, stop heating, cool and add 5mL water and heat to boiling, remove residual nitric acid-perchloric acid (if necessary, add water and boil once), continue heating until white smoke occurs, keep for 10 minutes, cool and transfer to a 100mL conical flask, and proceed as specified in 2.4 of GB/T8450-1987. 4.9 Determination of heavy metal content
4.9.1 Reagents and materials
4. 9. 1. 1 Sulfuric acid.
4.9.1.2 Hydrochloric acid.
4.9.1.3 Hydrochloric acid solution: 1+3.
4.9.1.4 Acetic acid solution: 1+3.
Ammonia solution: 1+2.
4. 9. 1. 5
Sodium sulfide solution: 100g/I.
4. 9. 1. 6
4.9.1.7 Lead standard solution (0.01mg/mL): Take 10mL of 0.1mg/mL lead standard solution in a 100mL volumetric flask and dilute to the mark.
4.9.2 Preparation of sample solution
Weigh 2.5g of carmine sample, accurate to 0.01g. 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 vapor no longer occurs. Place in an electric furnace 368
GB 4480.1-2001
, burn at 450~~550C until ash, then cool. Add 3mL of hydrochloric acid and shake well, then add 7mL of water and shake, 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. 4.9.3 Preparation of test solution
Measure 20mL of the sample solution and place it in a Nessler colorimetric tube. Add 1 drop of phenol test solution and add ammonia solution until the solution turns red. Then add 2mL of acetic acid solution. Filter if necessary, wash the filter paper with water, and add water to make it up to 50mL as the test solution. 4.9.4 Preparation of comparison solution
Measure 20mL of the blank test solution and place it in a Nessler colorimetric tube. Add 2.0mL and 1 drop of phenolic acid indicator solution, prepared in the same way as the test solution, as the comparison solution. Add 2 drops of sodium sulfide solution to the test solution and the comparison solution respectively, shake well and let 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 All items specified in this standard are factory inspections. 5.2 The quality inspection department of the production unit shall inspect the product quality of the food additive carmine in accordance with the provisions of this standard. The production unit shall ensure that the quality of all food additive carmine shipped meets the requirements of this standard and has a quality certificate in a certain format. 5.3 The food additive carmine is a batch of uniformly mixed products. 5.4 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 sample quickly and take out about 100g from it. 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. The manufacturer can sample and inspect the product that is evenly mixed before packaging, with the sampling amount of no less than 200g. 5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sample 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. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have firm and clear markings, including: "Food additives, product name, trademark, manufacturer name and address, quantity, gross weight, production date and batch number, shelf life. 6.2 Each bottle of product leaving the factory should have obvious markings, including: food additives, product name, manufacturer name and address, trademark, production and food hygiene license number, product promotion number and promotion name, shelf life, production date and batch number, net content, instructions for use. 6.3 The food additive carmine is packed in food-grade polyethylene plastic bottles, 0.5kg per bottle, and every 10 bottles are sealed in an outer box. Other forms of packaging The packaging can be determined by negotiation between the manufacturer and the user.
6.4 It must be protected from rain, moisture and sunlight during transportation and should be stored in a dry and cool warehouse. 6.5 This product must 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. If it is overdue, re-inspect whether it meets the requirements of this standard. It can still be used if it is qualified. 369
A1 Reagents and materials
A1.1 Hydrochloric acid.
A1.2 Ammonium ferrous sulfate.
A1.3 Ammonium thiocyanate solution: 200g/L
A1.4 Sulfuric acid solution: 1+1.
GB 4480. 1—2001
Appendix A
(Appendix of the standard)
Preparation of titanium trichloride standard titration solutionA1.5 Potassium dichromate standard solution: c(1/6KCr20,)=0.1mal/1. A2 Apparatus and equipment
See Figure 1 in the main text of this standard.
A3 Preparation of titanium trichloride standard titration solutionA3.1 Preparation: Take 100mL titanium trichloride solution and 75ml hydrochloric acid and place 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 lower-mouthed bottle and store under the protection of carbon dioxide gas. A3.2 Calibration: Weigh 3g of ammonium ferrous sulfate to an accuracy of 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 and continue to add 25mL of sulfuric acid solution below the liquid surface. With the protection of carbon dioxide gas flow, quickly and accurately add 45mL of potassium dichromate standard solution, then titrate with the titanium trichloride standard solution to be calibrated until it is close to the calculated end point, immediately add 25mL of ammonium thiocyanate solution, and continue to titrate with the titanium trichloride standard solution to be calibrated until the red color turns to green, which is the end point. The entire titration process should be carried out under the protection of carbon dioxide gas flow, and a blank test should be performed at the same time. A3.3 Expression of the concentration of titanium trichloride standard solution The concentration (c) of titanium trichloride standard solution is calculated according to formula (A1): C
Where; V,.--the volume of potassium dichromate standard solution, mL; Vic
V——the volume of titanium trichloride solution consumed by the potassium dichromate standard solution to be oxidized into high iron, mL: V:-.The volume of titanium trichloride solution consumed in the titration blank, mL; ci--the actual concentration of potassium dichromate standard solution, mal/L; Note: The above calibration needs to be performed immediately when analyzing the sample. 370
(A1)3 Expression of the concentration of titanium trichloride standard solution The concentration of titanium trichloride standard solution (c) is calculated according to formula (A1): C
Wherein; V,.--the volume of potassium dichromate standard solution, mL; Vic
V——the volume of titanium trichloride solution consumed by the potassium dichromate standard solution to oxidize into high iron, mL: V:-.The volume of titanium trichloride solution consumed in the titration blank, mL; ci--the actual concentration of potassium dichromate standard solution, mal/L; Note: The above calibration needs to be calibrated immediately when analyzing the sample. 370
(A1)3 Expression of the concentration of titanium trichloride standard solution The concentration of titanium trichloride standard solution (c) is calculated according to formula (A1): C
Wherein; V,.--the volume of potassium dichromate standard solution, mL; Vic
V——the volume of titanium trichloride solution consumed by the potassium dichromate standard solution to oxidize into high iron, mL: V:-.The volume of titanium trichloride solution consumed in the titration blank, mL; ci--the actual concentration of potassium dichromate standard solution, mal/L; Note: The above calibration needs to be calibrated immediately when analyzing the sample. 370
(A1)
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