Some standard content:
National Standard of the People's Republic of China
Food additives
Sodium cyclamate
Subject content and scope of application
GB 12488-1995
Replaces GB12488-90
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation, storage, etc. of the food additive sodium cyclamate (cyclamate).
This standard applies to sodium cyclamate prepared by reacting cyclohexylamine with chlorosulfonic acid or nitrogen sulfonic acid to synthesize cyclohexylaminosulfonic acid and then reacting with sodium hydroxide, which is used as a food sweetener. This product can be used in beverages, frozen drinks, cakes, candied fruits, prepared wines, pickles and pharmaceutical excipients, etc.
Molecular formula: C.H2NNaO,S·nH,O (crystalline product n=2, anhydrous product n=0)Structural formula:
-NHSO,Na
Relative molecular weight: crystalline product 237.24
Anhydrous product 201.22 (according to the 1991 international relative atomic mass) 2 Reference standards
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T 601
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 602
GB/T 603
Preparation of preparations and products used in test methods for chemical reagents GB/T 6284
GB/T 6678
GB/T 8450
GB/T8451
3 Product classification
General method for determination of moisture content in chemical products Gravimetric method General rules for sampling of chemical products
Determination of arsenic in food additives
Limit test method for heavy metals in food additives This product has type A and type B (containing two crystal waters), respectively called sodium cyclohexylaminosulfonate type A and sodium cyclohexylaminosulfonate type B. 4 Technical requirements
4.1 Appearance
Type A is white crystalline powder, needle-shaped crystals; Type B is white needle-shaped, flaky crystals; odorless, sweet. 4.2 The product should meet the requirements of the following table.
Approved by the State Bureau of Technical Supervision on August 17, 1995 and implemented on July 1, 1996
Sodium cyclohexylaminosulfonate (on dry basis), %Heating loss, %
Sulfate (as SO,), %
Arsenic (as As), %
Heavy metal (as Pb), %
GB12488—1995
Transparency (expressed as the transmittance of 100 g/L solution), % ≥Cyclohexylamine, %
Dicyclohexylamine
5 Test method
Meets the requirements
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and distilled water or water of corresponding purity. The standard solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
5.1 Identification test
5.1.1 Reagents and solutions
Ether;
Nitric acid;
Silver nitrate solution: 17g/L;
Sodium nitrite solution: 100g/L
Hydrochloric acid solution: 3-10;
Nitric acid solution: 3→50;
Barium chloride solution: 50g/L;
Sodium hydroxide solution: 50g/L.
5.1.2 Analysis steps
5.1.2.1 Take a platinum wire and dip it in a small amount of this product, burn it in a colorless flame, and the flame will appear yellow. 5.1.2.2 Take 3g of the sample, dissolve it in 20mL of water, take out 1mL, add 2mL of silver nitrate solution, and after 30s, a white precipitate of cyclohexylamino silver nitrate will be generated.
5.1.2.3 Take 0.3g of the sample, dissolve it in 20mL of water, add 5mL of sodium nitrite solution and 3mL of hydrochloric acid solution, heat it in a water bath for about 15min, take it out and cool it, then add 20mL of ether and shake it for extraction (after extraction, the water layer shall be subjected to the test in 5.1.2.4), put the ether layer into evaporator III, evaporate it in a water bath to remove the ether, then add 1mL of water and 0.5mL of nitric acid, heat it in a water bath for 20min, and evaporate it in a sand bath until it is dry without carbonization. After cooling, add 3mL of water to dissolve the residue, adjust the pH value to 4.5-7.0 with sodium hydroxide solution and nitric acid solution, and add 1mL of silver nitrate to generate a white precipitate. Add nitric acid to make it acidic, and the white precipitate will dissolve. 5.1.2.4 Take the water layer extracted with ether in 5.1.2.3, add 1 mL of barium chloride solution, and a white precipitate will be generated. 5.2 Determination of sodium cyclohexylaminosulfonate content
5.2.1 Summary of method
GB 12488-1995
Add glacial acetic acid to the sample after heating and dissolving, then cool to room temperature, and titrate with perchloric acid standard titration solution in the presence of crystal violet indicator solution until the solution changes from purple to blue-green. 5.2.2 Reagents and solutions
a. Glacial acetic acid;
b. Perchloric acid standard titration solution; c(HCIO.)=0.1 mol/L; c. Crystal violet indicator solution: 2 g/L. Weigh 0.2 g of crystal violet, dissolve it in glacial acetic acid, and dilute it to 100 mL with glacial acetic acid. 5.2.3 Analysis steps
Weigh 0.3 g (accurate to 0.0002 g) of the sample dried at 105°C for 2 h into a conical flask, add 30 mL of glacial acetic acid, heat to dissolve it, cool to room temperature, add 4 to 5 drops of crystal violet indicator solution, and titrate with standard perchloric acid solution until the solution changes from purple to blue-green, which is the end point. At the same time, perform a blank test.
5.2.4 Expression of analysis results
The content of sodium cyclohexylaminosulfonate (C.Hi2NNaO.S) expressed as mass percentage (X,) is calculated according to formula (1): X = AV×c×0.2012×100
the volume of perchloric acid standard titration solution consumed by the sample and the volume of perchloric acid standard titration solution consumed by the blank test Where: V—
difference, mL;
c-actual concentration of perchloric acid standard titration solution, mol/L; m
mass of sample, g;
the mass of sodium cyclohexylaminosulfonate equivalent to 1.00mL perchloric acid standard titration solution [c(HClO,)-1.000mol/L] expressed in grams.
5.2.5 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.3%. The arithmetic mean shall be taken as the analysis result. 5.2.6 Calibration
If the room temperature difference between the titration sample and the calibration of the perchloric acid standard titration solution exceeds 10℃, recalibration shall be performed. If it does not exceed 10℃, the concentration (c1) of the perchloric acid standard titration solution can be calibrated according to formula (2). C
c2 = 1 + 0. 001 1(t2 - t)
Where: 0.0011—expansion coefficient of glacial acetic acid;—room temperature when calibrating the perchloric acid standard titration solution, ℃; ti
t2——room temperature when titrating the sample, ℃; C2
-t,C is the concentration of the perchloric acid standard titration solution, mol/L. 5.3 Determination of heating loss
5.3.1 Summary of the method
The sample is dried in an oven to constant weight, and the adsorbed water, crystal water and volatile substances are lost. The loss is calculated by weighing. 5.3.2 Analysis steps
Weigh 2g of the sample (accurate to 0.0002g) into a weighing bottle with constant weight, dry it in a 105℃ constant temperature box for 2h, take it out and put it in a desiccator, cool it to room temperature and weigh it until constant weight. 5.3.3 Expression of analysis results
The heating loss (X,) expressed as mass percentage is calculated according to formula (3). 439
Where: mo-
mass of sample, g,
GB 12488-1995
(m - m2) × 100
mass of weighing bottle and sample before drying, g: mass of weighing bottle and sample after drying, g. 5.3.4 Allowable difference
The difference between two parallel determination results shall not exceed 0.1%, and the arithmetic mean shall be taken as the analysis result. 5.4 pH value
Weigh 10g of the sample (accurate to 0.1g), dissolve it in freshly boiled and cooled water, and dilute to 100mL, and measure it with an acidometer. 5.5 Determination of sulfate content
5.5.1 Reagents and solutions
a. 95% ethanol;
Hydrochloric acid solution: 3-10;
c. Barium chloride solution: 250g/L;
d. Sulfate standard solution (each 1mL contains 0.1mgSO,). 5.5.2 Analysis steps
(3)
Weigh 1g of the sample (accurate to 0.01g), dissolve it in about 40mL of water, place it in a 100mL volumetric flask (filter if necessary), dilute it with water to the mark, shake it well, accurately take 10mL of the above solution, place it in a 25mL colorimetric tube, add 5mL of 95% ethanol and 1mL of hydrochloric acid solution, add 3mL of sodium chloride solution under shaking, dilute it with water to 25mL, shake it well, and let it stand for 10min. The turbidity should not be greater than the standard. The standard is to take 0.5mL of sulfate standard solution and treat it in the same way as the sample. 5.6 Determination of arsenic content
Determine it according to the arsenic spot method in GB/T8450. Arsenic standard solution, each milliliter contains 0.001mg arsenic. 5.7 Determination of heavy metal content
Determine it according to the hydrogen sulfide method in GB/T8451. Lead standard solution, each milliliter contains 0.01mgPb. 5.8 Determination of transparency
Weigh 2.50g of the sample (accurate to 0.01g), place it in a 25mL volumetric flask, add water to dissolve, dilute to the scale, and shake. Use a spectrophotometer to measure its transmittance at a wavelength of 420nm in a 1cm absorption cell. The transmittance of water is 100%. 5.9 Determination of cyclohexylamine content
5.9.1 Reagents and solutions
a Alkaline disodium ethylenediaminetetraacetic acid solution: weigh 10g disodium ethylenediaminetetraacetic acid and 3.4g sodium hydroxide, add water to dissolve, and dilute to 100mL with water.
Methyl orange boric acid solution: weigh 200mg methyl orange and 3.5g boric acid, add 100mL water, heat in a water bath to dissolve, and let stand for more than 24h, filter before use.
c. Mixture of chloroform and n-butanol: 20+1. d.
Methanol and sulfuric acid mixture: 50+1.
Cyclohexylamine standard solution: each milliliter contains 0.0025mg cyclohexylamine. Weigh 0.1g cyclohexylamine (accurate to 0.0002g), place it in a 100mL volumetric flask, add 50mL water and 0.5mL hydrochloric acid, dissolve it, dilute it with water to the mark, and shake it well. Accurately measure 5.0mL, place it in another 100mL volumetric flask, dilute it with water to the mark, and shake it. Accurately measure 5.0mL of this dilution, place it in a 100mL volumetric flask, dilute it with water to the mark, and shake it.
5.9.2 Analysis steps
GB12488--1995
Weigh 10 g of the sample (accurate to 0.1 g), place it in a 100 mL volumetric flask, add water to dissolve, dilute with water to the scale, and shake well. Accurately pipette 10mL of the above solution and cyclohexylamine standard solution, place them in 60mL separatory funnels, add 3.0mL of alkaline ethylenediaminetetraacetic acid disodium salt solution, 15.0mL of chloroform and n-butanol mixture, shake for 2min, let stand, separate the fluoroform layer, measure 10.0mL of fluoroform extract, place in another 60mL separatory funnel, add 2.0mL of methyl orange acid solution, shake for 2min, let stand, separate the chloroform layer, add 1g of anhydrous sodium sulfate, shake, let stand, measure 5.0mL of chloroform solution, place in colorimetric tubes, add 0.5mL of methanol and sulfuric acid mixture, and spread evenly. The color of the sample solution shall not be darker than the standard. 5.10 Determination of dicyclohexylamine content
5.10.1 Reagents and solutions
Chloroform: Wash three times with water, each time using 1/3 of the amount of water used for chloroform, and separate the chloroform layer for determination; a.
Sodium hydroxide solution: 40g/L;
Sodium bicarbonate solution: 8.4g/L;
Hydrochloric acid solution: 1→12;
Reagent A: Weigh 75mg of bromophenol blue, add 60mL of water, add 10mL of sodium bicarbonate solution, stir to dissolve, adjust the pH value to 4.0 with hydrochloric acid solution, dilute to 100mlL with water, shake well, store in a cool and dark place, and use within 48h; f.
Reagent B: Measure 20mL of hydrochloric acid solution (1-→12) and 16.6rmL of glacial acetic acid in a 100mL volumetric flask, dilute to the scale with water, and shake well.
5.10.2 Instruments
Spectrophotometer, 5cm absorption cell;
Separatory funnel, 250ml.
5.10.3 Analysis steps
Weigh 10.0g of the sample (accurate to 0.01g) into a 250mL separatory funnel, add 100mL of water to dissolve it, and measure 100ml of water into another separatory funnel as a reagent blank. Add 10mL of sodium hydroxide solution to each, and then extract with 10, 5, and 5mL of trifluoromethane respectively, respectively, combine the trichloromethane extracts into two other separatory funnels, add 100mL of water, 3.0mL of reagent B, and 1.0mL of reagent A to each, shake for 3min, place in the dark for 30min, let stand for stratification, separate the trichloromethane layer into a 25mL colorimetric tube, and add trichloromethane to 25mL. At a wavelength of 410nm, use a 5cm absorption cell and adjust to zero with chloroform to measure the absorbance of the reagent blank and the sample solution. The difference in absorbance is no more than 0.20 to meet the requirements.
6 Inspection rules
6.1 All technical indicators listed in this standard are type inspection items. Under normal production conditions, type inspection is carried out every six months, of which 5.2, 5.3, 5.4, 5.5, 5.6, 5.7, 5.8 and other seven items are factory inspection items. 6.2 This product should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer guarantees that all products shipped meet the requirements of this standard. Each batch of products shipped should be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user can conduct quality inspection on the received products according to the inspection rules and methods specified in this standard. 6.4 The product is one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the name of the manufacturer, product name, batch number, specifications, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one indicator does not meet the standard during the inspection, it shall be re-verified from twice the amount of packaging. If the result of the re-inspection of the product is that even if only one indicator does not meet the standard, the entire batch shall be unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use and is sealed. The outer packaging is a paper barrel or a propylene woven bag that is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or harmful substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Institute of Chemical Industry and Food Hygiene Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd. and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclamate". 4427 Determination of heavy metal content
Determination shall be carried out according to the hydrogen sulfide method of GB/T8451. Lead standard solution, containing 0.01 mgPb per milliliter. 5.8 Determination of transparency
Weigh 2.50 g of the sample (accurate to 0.01 g), place it in a 25 mL volumetric flask, add water to dissolve, dilute to the scale, and shake the hook. Use a spectrophotometer to measure its transmittance at a wavelength of 420 nm in a 1 cm absorption cell. The transmittance of water is 100%. 5.9 Determination of cyclohexylamine content
5.9.1 Reagents and solutions
a Alkaline disodium ethylenediaminetetraacetic acid solution: Weigh 10 g disodium ethylenediaminetetraacetic acid and 3.4 g sodium hydroxide, add water to dissolve, and dilute to 100 mL with water.
Methyl orange boric acid solution: weigh 200mg methyl orange and 3.5g boric acid, add 100mL water, heat in a water bath to dissolve, and let stand for more than 24h, filter before use.
c. Chloroform and n-butanol mixture: 20+1. d.
Methanol and sulfuric acid mixture: 50+1.
Cyclohexylamine standard solution: 0.0025mg cyclohexylamine per milliliter. Weigh 0.1g cyclohexylamine (accurate to 0.0002g), place in a 100mL volumetric flask, add 50mL water and 0.5mL hydrochloric acid, dilute to scale with water after dissolution, and shake well. Accurately measure 5.0mL, place in another 100mL volumetric flask, dilute to scale with water, and shake to hook. Accurately measure 5.0mL of this dilution, place in a 100mL volumetric flask, dilute to scale with water, and shake to hook.
5.9.2 Analysis steps
GB12488--1995
Weigh 10 g of the sample (accurate to 0.1 g), place it in a 100 mL volumetric flask, add water to dissolve, dilute with water to the scale, and shake well. Accurately pipette 10mL of the above solution and cyclohexylamine standard solution, place them in 60mL separatory funnels, add 3.0mL of alkaline ethylenediaminetetraacetic acid disodium salt solution, 15.0mL of chloroform and n-butanol mixture, shake for 2min, let stand, separate the fluoroform layer, measure 10.0mL of fluoroform extract, place in another 60mL separatory funnel, add 2.0mL of methyl orange acid solution, shake for 2min, let stand, separate the chloroform layer, add 1g of anhydrous sodium sulfate, shake, let stand, measure 5.0mL of chloroform solution, place in colorimetric tubes, add 0.5mL of methanol and sulfuric acid mixture, and spread evenly. The color of the sample solution shall not be darker than the standard. 5.10 Determination of dicyclohexylamine content
5.10.1 Reagents and solutions
Chloroform: Wash three times with water, each time using 1/3 of the amount of water used for chloroform, and separate the chloroform layer for determination; a.
Sodium hydroxide solution: 40g/L;
Sodium bicarbonate solution: 8.4g/L;
Hydrochloric acid solution: 1→12;
Reagent A: Weigh 75mg of bromophenol blue, add 60mL of water, add 10mL of sodium bicarbonate solution, stir to dissolve, adjust the pH value to 4.0 with hydrochloric acid solution, dilute to 100mlL with water, shake well, store in a cool and dark place, and use within 48h; f.
Reagent B: Measure 20mL of hydrochloric acid solution (1-→12) and 16.6rmL of glacial acetic acid in a 100mL volumetric flask, dilute to the scale with water, and shake well.
5.10.2 Instruments
Spectrophotometer, 5cm absorption cell;
Separatory funnel, 250ml.
5.10.3 Analysis steps
Weigh 10.0g of the sample (accurate to 0.01g) into a 250mL separatory funnel, add 100mL of water to dissolve it, and measure 100ml of water into another separatory funnel as a reagent blank. Add 10mL of sodium hydroxide solution to each, and then extract with 10, 5, and 5mL of trifluoromethane respectively, respectively, combine the trichloromethane extracts into two other separatory funnels, add 100mL of water, 3.0mL of reagent B, and 1.0mL of reagent A to each, shake for 3min, place in the dark for 30min, let stand for stratification, separate the trichloromethane layer into a 25mL colorimetric tube, and add trichloromethane to 25mL. At a wavelength of 410nm, use a 5cm absorption cell and adjust to zero with chloroform to measure the absorbance of the reagent blank and the sample solution. The difference in absorbance is no more than 0.20 to meet the requirements.
6 Inspection rules
6.1 All technical indicators listed in this standard are type inspection items. Under normal production conditions, type inspection is carried out every six months, of which 5.2, 5.3, 5.4, 5.5, 5.6, 5.7, 5.8 and other seven items are factory inspection items. 6.2 This product should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer guarantees that all products shipped meet the requirements of this standard. Each batch of products shipped should be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user can conduct quality inspection on the received products according to the inspection rules and methods specified in this standard. 6.4 The product is one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the name of the manufacturer, product name, batch number, specifications, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one indicator does not meet the standard during the inspection, it shall be re-verified from twice the amount of packaging. If the result of the re-inspection of the product is that even if only one indicator does not meet the standard, the entire batch shall be unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use and is sealed. The outer packaging is a paper barrel or a propylene woven bag that is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or harmful substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Institute of Chemical Industry and Food Hygiene Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd. and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclamate". 4427 Determination of heavy metal content
Determination shall be carried out according to the hydrogen sulfide method of GB/T8451. Lead standard solution, containing 0.01 mgPb per milliliter. 5.8 Determination of transparency
Weigh 2.50 g of the sample (accurate to 0.01 g), place it in a 25 mL volumetric flask, add water to dissolve, dilute to the scale, and shake the hook. Use a spectrophotometer to measure its transmittance at a wavelength of 420 nm in a 1 cm absorption cell. The transmittance of water is 100%. 5.9 Determination of cyclohexylamine content
5.9.1 Reagents and solutions
a Alkaline disodium ethylenediaminetetraacetic acid solution: Weigh 10 g disodium ethylenediaminetetraacetic acid and 3.4 g sodium hydroxide, add water to dissolve, and dilute to 100 mL with water.
Methyl orange boric acid solution: weigh 200mg methyl orange and 3.5g boric acid, add 100mL water, heat in a water bath to dissolve, and let stand for more than 24h, filter before use.
c. Chloroform and n-butanol mixture: 20+1. d.
Methanol and sulfuric acid mixture: 50+1.
Cyclohexylamine standard solution: 0.0025mg cyclohexylamine per milliliter. Weigh 0.1g cyclohexylamine (accurate to 0.0002g), place in a 100mL volumetric flask, add 50mL water and 0.5mL hydrochloric acid, dilute to scale with water after dissolution, and shake well. Accurately measure 5.0mL, place in another 100mL volumetric flask, dilute to scale with water, and shake to hook. Accurately measure 5.0mL of this dilution, place in a 100mL volumetric flask, dilute to scale with water, and shake to hook.
5.9.2 Analysis steps
GB12488--1995
Weigh 10 g of the sample (accurate to 0.1 g), place it in a 100 mL volumetric flask, add water to dissolve, dilute with water to the scale, and shake well. Accurately pipette 10mL of the above solution and cyclohexylamine standard solution, place them in 60mL separatory funnels, add 3.0mL of alkaline ethylenediaminetetraacetic acid disodium salt solution, 15.0mL of chloroform and n-butanol mixture, shake for 2min, let stand, separate the fluoroform layer, measure 10.0mL of fluoroform extract, place in another 60mL separatory funnel, add 2.0mL of methyl orange acid solution, shake for 2min, let stand, separate the chloroform layer, add 1g of anhydrous sodium sulfate, shake, let stand, measure 5.0mL of chloroform solution, place in colorimetric tubes, add 0.5mL of methanol and sulfuric acid mixture, and spread evenly. The color of the sample solution shall not be darker than the standard. 5.10 Determination of dicyclohexylamine content
5.10.1 Reagents and solutions
Chloroform: Wash three times with water, each time using 1/3 of the amount of water used for chloroform, and separate the chloroform layer for determination; a.
Sodium hydroxide solution: 40g/L;
Sodium bicarbonate solution: 8.4g/L;
Hydrochloric acid solution: 1→12;
Reagent A: Weigh 75mg of bromophenol blue, add 60mL of water, add 10mL of sodium bicarbonate solution, stir to dissolve, adjust the pH value to 4.0 with hydrochloric acid solution, dilute to 100mlL with water, shake well, store in a cool and dark place, and use within 48h; f.
Reagent B: Measure 20mL of hydrochloric acid solution (1-→12) and 16.6rmL of glacial acetic acid in a 100mL volumetric flask, dilute to the scale with water, and shake well.
5.10.2 Instruments
Spectrophotometer, 5cm absorption cell;
Separatory funnel, 250ml.
5.10.3 Analysis steps
Weigh 10.0g of the sample (accurate to 0.01g) into a 250mL separatory funnel, add 100mL of water to dissolve it, and measure 100ml of water into another separatory funnel as a reagent blank. Add 10mL of sodium hydroxide solution to each, and then extract with 10, 5, and 5mL of trifluoromethane respectively, respectively, combine the trichloromethane extracts into two other separatory funnels, add 100mL of water, 3.0mL of reagent B, and 1.0mL of reagent A to each, shake for 3min, place in the dark for 30min, let stand for stratification, separate the trichloromethane layer into a 25mL colorimetric tube, and add trichloromethane to 25mL. At a wavelength of 410nm, use a 5cm absorption cell and adjust to zero with chloroform to measure the absorbance of the reagent blank and the sample solution. The difference in absorbance is no more than 0.20 to meet the requirements.
6 Inspection rules
6.1 All technical indicators listed in this standard are type inspection items. Under normal production conditions, type inspection is carried out every six months, of which 5.2, 5.3, 5.4, 5.5, 5.6, 5.7, 5.8 and other seven items are factory inspection items. 6.2 This product should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer guarantees that all products shipped meet the requirements of this standard. Each batch of products shipped should be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user can conduct quality inspection on the received products according to the inspection rules and methods specified in this standard. 6.4 The product is one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the name of the manufacturer, product name, batch number, specifications, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one indicator does not meet the standard during the inspection, it shall be re-verified from twice the amount of packaging. If the result of the re-inspection of the product is that even if only one indicator does not meet the standard, the entire batch shall be unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use and is sealed. The outer packaging is a paper barrel or a propylene woven bag that is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or harmful substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Institute of Chemical Industry and Food Hygiene Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd. and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclamate". 4420mL, put it in a 100mL volumetric flask, dilute it with water to the mark, and shake it.
5.9.2 Analysis steps
GB12488--1995
Weigh 10g of the sample (accurate to 0.1g), put it in a 100mL volumetric flask, add water to dissolve, and dilute it with water to the mark, and shake it well. Accurately pipette 10mL of the above solution and cyclohexylamine standard solution, place them in 60mL separatory funnels, add 3.0mL of alkaline ethylenediaminetetraacetic acid disodium salt solution, 15.0mL of chloroform and n-butanol mixture, shake for 2min, let stand, separate the fluoroform layer, measure 10.0mL of fluoroform extract, place in another 60mL separatory funnel, add 2.0mL of methyl orange acid solution, shake for 2min, let stand, separate the chloroform layer, add 1g of anhydrous sodium sulfate, shake, let stand, measure 5.0mL of chloroform solution, place in colorimetric tubes, add 0.5mL of methanol and sulfuric acid mixture, and spread evenly. The color of the sample solution shall not be darker than the standard. 5.10 Determination of dicyclohexylamine content
5.10.1 Reagents and solutions
Chloroform: Wash three times with water, each time using 1/3 of the amount of water used for chloroform, and separate the chloroform layer for determination; a.
Sodium hydroxide solution: 40g/L;
Sodium bicarbonate solution: 8.4g/L;
Hydrochloric acid solution: 1→12;
Reagent A: Weigh 75mg of bromophenol blue, add 60mL of water, add 10mL of sodium bicarbonate solution, stir to dissolve, adjust the pH value to 4.0 with hydrochloric acid solution, dilute to 100mlL with water, shake well, store in a cool and dark place, and use within 48h; f.
Reagent B: Measure 20mL of hydrochloric acid solution (1-→12) and 16.6rmL of glacial acetic acid in a 100mL volumetric flask, dilute to the scale with water, and shake well. bzxZ.net
5.10.2 Instruments
Spectrophotometer, 5cm absorption cell;
Separatory funnel, 250ml.
5.10.3 Analysis steps
Weigh 10.0g of the sample (accurate to 0.01g) into a 250mL separatory funnel, add 100mL of water to dissolve it, and measure 100ml of water into another separatory funnel as a reagent blank. Add 10mL of sodium hydroxide solution to each, and then extract with 10, 5, and 5mL of trifluoromethane respectively, respectively, combine the trichloromethane extracts into two other separatory funnels, add 100mL of water, 3.0mL of reagent B, and 1.0mL of reagent A to each, shake for 3min, place in the dark for 30min, let stand for stratification, separate the trichloromethane layer into a 25mL colorimetric tube, and add trichloromethane to 25mL. At a wavelength of 410nm, use a 5cm absorption cell and adjust to zero with chloroform to measure the absorbance of the reagent blank and the sample solution. The difference in absorbance is no more than 0.20 to meet the requirements.
6 Inspection rules
6.1 All technical indicators listed in this standard are type inspection items. Under normal production conditions, type inspection is carried out every six months, of which 5.2, 5.3, 5.4, 5.5, 5.6, 5.7, 5.8 and other seven items are factory inspection items. 6.2 This product should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer guarantees that all products shipped meet the requirements of this standard. Each batch of products shipped should be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user can conduct quality inspection on the received products according to the inspection rules and methods specified in this standard. 6.4 The product is one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the name of the manufacturer, product name, batch number, specifications, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one indicator does not meet the standard during the inspection, it shall be re-verified from twice the amount of packaging. If the result of the re-inspection of the product is that even if only one indicator does not meet the standard, the entire batch shall be unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use and is sealed. The outer packaging is a paper barrel or a propylene woven bag that is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or harmful substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Institute of Chemical Industry and Food Hygiene Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd. and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclamate". 4420mL, put it in a 100mL volumetric flask, dilute it with water to the mark, and shake it.
5.9.2 Analysis steps
GB12488--1995
Weigh 10g of the sample (accurate to 0.1g), put it in a 100mL volumetric flask, add water to dissolve, and dilute it with water to the mark, and shake it well. Accurately pipette 10mL of the above solution and cyclohexylamine standard solution, place them in 60mL separatory funnels, add 3.0mL of alkaline ethylenediaminetetraacetic acid disodium salt solution, 15.0mL of chloroform and n-butanol mixture, shake for 2min, let stand, separate the fluoroform layer, measure 10.0mL of fluoroform extract, place in another 60mL separatory funnel, add 2.0mL of methyl orange acid solution, shake for 2min, let stand, separate the chloroform layer, add 1g of anhydrous sodium sulfate, shake, let stand, measure 5.0mL of chloroform solution, place in colorimetric tubes, add 0.5mL of methanol and sulfuric acid mixture, and spread evenly. The color of the sample solution shall not be darker than the standard. 5.10 Determination of dicyclohexylamine content
5.10.1 Reagents and solutions
Chloroform: Wash three times with water, each time using 1/3 of the amount of water used for chloroform, and separate the chloroform layer for determination; a.
Sodium hydroxide solution: 40g/L;
Sodium bicarbonate solution: 8.4g/L;
Hydrochloric acid solution: 1→12;
Reagent A: Weigh 75mg of bromophenol blue, add 60mL of water, add 10mL of sodium bicarbonate solution, stir to dissolve, adjust the pH value to 4.0 with hydrochloric acid solution, dilute to 100mlL with water, shake well, store in a cool and dark place, and use within 48h; f.
Reagent B: Measure 20mL of hydrochloric acid solution (1-→12) and 16.6rmL of glacial acetic acid in a 100mL volumetric flask, dilute to the scale with water, and shake well.
5.10.2 Instruments
Spectrophotometer, 5cm absorption cell;
Separatory funnel, 250ml.
5.10.3 Analysis steps
Weigh 10.0g of the sample (accurate to 0.01g) into a 250mL separatory funnel, add 100mL of water to dissolve it, and measure 100ml of water into another separatory funnel as a reagent blank. Add 10mL of sodium hydroxide solution to each, and then extract with 10, 5, and 5mL of trifluoromethane respectively, respectively, combine the trichloromethane extracts into two other separatory funnels, add 100mL of water, 3.0mL of reagent B, and 1.0mL of reagent A to each, shake for 3min, place in the dark for 30min, let stand for stratification, separate the trichloromethane layer into a 25mL colorimetric tube, and add trichloromethane to 25mL. At a wavelength of 410nm, use a 5cm absorption cell and adjust to zero with chloroform to measure the absorbance of the reagent blank and the sample solution. The difference in absorbance is no more than 0.20 to meet the requirements.
6 Inspection rules
6.1 All technical indicators listed in this standard are type inspection items. Under normal production conditions, type inspection is carried out every six months, of which 5.2, 5.3, 5.4, 5.5, 5.6, 5.7, 5.8 and other seven items are factory inspection items. 6.2 This product should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer guarantees that all products shipped meet the requirements of this standard. Each batch of products shipped should be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user can conduct quality inspection on the received products according to the inspection rules and methods specified in this standard. 6.4 The product is one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the name of the manufacturer, product name, batch number, specifications, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one indicator does not meet the standard during the inspection, it shall be re-verified from twice the amount of packaging. If the result of the re-inspection of the product is that even if only one indicator does not meet the standard, the entire batch shall be unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use and is sealed. The outer packaging is a paper barrel or a propylene woven bag that is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or harmful substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Institute of Chemical Industry and Food Hygiene Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd. and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclamate". 4427, 5.8 and other seven items are factory inspection items. 6.2 This product shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user unit may conduct quality inspection on the received products in accordance with the inspection rules and methods specified in this standard. 6.4 The product is considered as one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the manufacturer name, product name, batch number, specification, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one of the indicators does not meet the standard during the inspection, it should be re-inspected from twice the amount of packaging. If only one indicator does not meet the standard after the re-inspection of the product, the entire batch will be considered unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use, which is sealed, and the outer packaging is a paper barrel or a propylene woven bag, which is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or hazardous substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Chemical Industry Research Institute and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Supervision and Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd., and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping, and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclohexylaminosulfonate". 4427, 5.8 and other seven items are factory inspection items. 6.2 This product shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality manual. Its contents include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date, and shelf life. 6.3 The user unit may conduct quality inspection on the received products in accordance with the inspection rules and methods specified in this standard. 6.4 The product is considered as one batch per feeding.
6.5 The sampling quantity of each batch of products shall be carried out in accordance with the provisions of 6.6 of GB/T6678, and the total sample of each batch shall not be less than 100g. The selected samples shall be quickly mixed, divided into bottles (bags), and labels shall be affixed to the bottles (bags), indicating the manufacturer name, product name, batch number, specification, sampling date and name of the sampler. One bottle (bag) shall be sent to the inspection department for inspection, and the other bottle (bag) shall be sealed and stored for two years for future reference. 6.6 If one of the indicators does not meet the standard during the inspection, it should be re-inspected from twice the amount of packaging. If only one indicator does not meet the standard after the re-inspection of the product, the entire batch will be considered unqualified. 6.7 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 7 Marking, packaging, transportation and storage
7.1 The inner and outer packaging should be marked with the product name, manufacturer name, factory address, trademark, production license number, net weight, standard code, batch number, production date, shelf life, and the words "food additive". GB12488-1995
7.2 The inner packaging of this product is a plastic bag that meets the requirements of food use, which is sealed, and the outer packaging is a paper barrel or a propylene woven bag, which is sealed tightly. The packaging unit is 1, 15, 25kg or packaged according to user requirements. 7.3 This product should be stored in a dry place to prevent moisture. 7.4 This product must not be mixed or transported with toxic or hazardous substances. 7.5 This product has a shelf life of two years if it meets the storage requirements and the packaging is intact. If the sampling test results still meet the requirements of this standard after two years, it can still be used.
Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Chemical Industry Research Institute and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Zhongshan Food Additive Factory, Guangdong Food Hygiene Supervision and Inspection Institute, Guangdong Shenzhen Fangda Additive Co., Ltd., and Guangzhou Pharmaceutical Industry Research Institute.
The main drafters of this standard are Hao Zhicheng, Jiang Yuebi, Wen Huiping, and She Peizhu. This standard was first issued and implemented on June 1, 1991. This standard is equivalent to the United Nations Food and Agriculture Organization/World Health Organization Joint Expert Committee on Food Additives (FAO/WHOJECFA) CXAS-1983 "Sodium Cyclohexylaminosulfonate". 442
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