This standard is applicable to the food additive ethyl p-hydroxybenzoate vinegar which is esterified by p-hydroxybenzoic acid and ethanol with sulfuric acid as catalyst. The product is used as preservative in food, medicine and cosmetics.
Molecular formula: C9H 1003
Building type:
Relative molecular mass: 166. 18 (according to international relative atomic mass 200 1). The clauses in the following documents become the clauses of this standard by reference. All subsequent modifications (excluding errata) or revisions of dated reference documents are not applicable to this standard. However, parties who have reached an agreement according to this standard are encouraged to study whether the latest versions of these documents can be used. For undated reference documents, the latest edition is applicable to this standard.
GB /T 1 9 1 Graphic signs for packaging, storage and transportation (GB/T 19 1-2000, ISO 780；; 1997)
Preparation of GB /T 6 0 1 Standard Titration Solution for Chemical Reagents
GB /T 602 Preparation of standard solution for impurity determination of chemical reagents (GB/T 602-2002, ISO 6353-1; 1982，NEQ)
Preparation of preparations and products used in GB /T 603 test methods for chemical reagents (GB/T 603-2002, NEQ ISO 6353-1:1982).
GB /T 6 17 general method for measuring melting point range of chemical reagents
GB /T 5009.76 determination of arsenic in food additives
General rules for sampling of chemical products
GB /T 6 679 general rules for sampling solid chemical products
GB /T 6 682 Specifications and test methods for water used in analytical laboratories (GB/T 6682- 1992, ISO 3696: 65438 standard +0987)
GB /T 9724- 1988 general rules for determination of pH value of chemical reagents
GB /T 974 1 General method for determination of chemical reagent residue on ignition 3. 1 Characteristics: white crystalline powder, odorless or slightly peculiar smell, slightly bitter and burning.
3.2 The food additive ethyl p-hydroxybenzoate shall meet the technical requirements shown in Table 1.
Table 1 technical requirements: the mass fraction of ethyl p-hydroxybenzoate (calculated on dry basis) is 99.0- 100.5%, the melting point is 16- 18℃, and the mass fraction of free acid (calculated on p-hydroxybenzoic acid) is ≤0.55%. The mass fraction of dry reduction is ≤0.50%, the mass fraction of residue on ignition is ≤0.05%, the mass fraction of arsenic is ≤ 1ppm, and the mass fraction of heavy metals is ≤ 10ppm. Note: The mass fraction of arsenic and heavy metals (calculated by lead) is mandatory. 4. 1. Display
Some test procedures specified in the test methods may lead to dangerous situations. Operators should take appropriate safety and health measures.
4.2 General provisions
Unless otherwise specified, only reagents identified as analytically pure or tertiary water in GB/T 6682 are used in the analysis. Unless otherwise specified, the standard titration solution, impurity determination standard solution, preparations and products used in the analysis are prepared according to GB/T 60 1, GB/T 602 and GB/T 603.
4.3 Identification test
4.3. 1 reagent
4.3. 1. 1 sodium hydroxide solution: 40g/l;
4.3. 1.2 barium chloride solution: 250g/l;
4.3. 1.3 sodium hydroxide solution: 80g/l;
4.3. 1.4 sulfuric acid solution:1-17;
4.3. 1.5 iodine solution:12.7g/L.
4.3.2 Identification method
4.3.2. 1 Weigh about 0.5 g of laboratory sample, accurate to 0.0 1 g, add 10m L of sodium hydroxide solution (4.3. 1. 1), boil for 30min, and evaporate to about 5 mL. Then the precipitate was dried at 105℃ and 2℃, and the melting point was determined according to GB/T 6 17, and its final melting temperature should be within the range of 2 13℃-2 17℃.
4.3.2.2 weighed 0.5g of laboratory sample, accurate to 0.0 1 g, added 5ml of sodium hydroxide solution (4.3. 1.3), heated in a boiling water bath for 5min, added 6ml of sulfuric acid solution, cooled and filtered, and added 5ml of sodium hydroxide solution (4.3. 1.3) to the filtrate.
4.4 Determination of Ethyl Benzoate and Acetate in Light Tomb
4.4. 1 method summary
The sample is saponified with a certain amount of sodium hydroxide, the excess sodium hydroxide is titrated with sulfuric acid standard titration solution, and the end point is indicated by an acidity meter. According to the consumed volume of sulfuric acid standard titration solution, the content of ethyl p-hydroxybenzoate was calculated.
4.4.2 Reagent
4.4.2. 1 sodium hydroxide solution: 40g/l;
4.4.2.2 buffer solution: buffer solution with pH of 4.0 1 and 6.86 at 25℃ prepared according to 4.3 and 4.4 in GB/T 9724- 1988;
4.4.2.3 sulfuric acid standard titration solution: c (1/2hzso4) =1mol/l.
instrument
PH acidimeter: the accuracy is 0. 1 pH unit.
4.4.4 Analysis Steps
4.4.4. 1 debug the acidity meter according to GB/T 9724.
4.4.4.2 weighed about 2g samples dried at 80℃ and 2℃ for 2h, and the accuracy was 0. 000 2 g, put it in a 250 mL iodine volumetric flask, add 40 mL sodium hydroxide solution accurately, slowly heat it to boiling, reflux it for 65438 0 h, cool it to room temperature, quantitatively transfer it to a beaker, transfer it to a pH meter adjusted with buffer solution with pH=6.86 in advance, and titrate it with sulfuric acid standard titration solution.
4.4.4.3 in the determination at the same time, according to the same steps as the determination, without adding samples and using the same amount of reagent solution to do a blank test.
4.4.5 Calculation of results
The mass fraction w of ethyl terephthalate (C9H 1003) is expressed in%, and calculated according to the formula (1):
Among them:
V—— the volume value of sulfuric acid standard titration solution (4.4.2.3) consumed in blank test, in milliliter (ml);
Volume value of sulfuric acid standard titration solution (4.4.2.3) consumed by the sample, in milliliter (ml);
C the accurate value of the concentration of sulfuric acid standard titration solution, in mol/l;
M refers to the numerical value of sample mass, and the unit is gram (g);
M is the numerical value of the molar mass of ethyl p-benzoate, and the unit is gram per mole (g/mol) (m =166.2) a.
Take the arithmetic average of the two parallel determination results as the determination result, and the absolute difference between the two parallel determination results is not more than 0.2000.
4.5 Determination of melting point
4.5. 1 capillary method (arbitration method)
According to G B/ T 6 17. The final melting temperature is taken as the determination result. Take the arithmetic average of two times as the determination result, and the absolute difference between the two parallel determination results is not more than 0.30C C C.
4.5.2 Digital melting point instrument method
4.5.2. 1 instrument
Digital melting point instrument: temperature control accuracy is 0.50C C.
4.5.2.2 analysis steps
Adjust and correct the melting point instrument according to its operating instructions. Adjust the temperature of the instrument to 1 12 * C, grind the dried sample and put it into a clean and dry melting point tube. Take a dry hollow glass tube about 800 mm long and stand upright on a glass or porcelain plate. Drop the melting point tube with the sample for more than 65,438+05 times until the sample on the melting point tube shrinks to a height of 3 mm-5 mm or a suitable height. When the temperature of the instrument is stable, insert the melting point tube containing the sample into the injection hole and adjust the zero point at the rate of 10C/min.
The average value of the two parallel determination results is taken as the determination result, and the absolute difference between the two parallel determination results is not more than 0.50℃.
4.6 Determination of F in Free Acid
4.6. 1 reagent
4.6. 1. 1 sodium hydroxide standard titration solution: c (NaOH) = 0.1mol/l;
4.6. 1.2 methyl red indicator: 1 g/l.
4.6.2 Analysis Steps
Weight 0. 7 5g laboratory sample, accurate to 0.0 1g, put in 15m L hot water at about 80℃, heat 1 min, cool, filter, take 10 mL filtrate, add 2 drops of methyl red indicator, titrate to yellow with sodium hydroxide standard titration solution, and stabilize for 30 s.
4.7 Determination of F in Sulfate
4.7. 1 reagent
4.7. 1. 1 hydrochloric acid solution:1.13;
4.7. 1.2 barium chloride solution: 250g/l;
4.7. 1.3 sulfate (so,) standard solution: 0. 1 mg/ml,
4.7.2 Analysis Steps
Weight 1. 0 g of laboratory sample, accurate to 0.065438 0 g, add 65438 000 ml of hot water, shake well, heat for 5 minutes, cool, add water to 65438 000 ml, filter, take 40 ml of filtrate in a 50 ml colorimetric tube, add 5 ml of hydrochloric acid solution and 3 ml of barium chloride solution, and shake well. The standard is to take 0.9-6 ml standard solution of sulfuric acid (504) in a 50 ml colorimetric tube and treat it with 40 ml sample filtrate.
4.8 Determination of dry operation minus F
4.8. 1 analysis steps
Weigh 2g laboratory samples, accurate to 0.00±02g, and put them in a weighing bottle with a diameter of 45mm and a height of 25 mm. The weighing bottle has been dried at 80℃ and 2℃ in advance until the quality is constant and evenly distributed, dried at 80℃ and 2℃ for 2h, taken out, cooled to room temperature and weighed.
Calculation of results
The mass fraction w2 of drying weight loss is expressed as%, and calculated according to Formula (2):
Among them:
M—— the numerical value of sample mass before drying, with the unit of g;
Ml—— the numerical value of the dried sample mass, with the unit of gram (9).
Take the arithmetic average of the two parallel determination results as the determination result, and the absolute difference between the two parallel determination results is not more than 0.05%.
4.9 Determination of residue on ignition
According to GB /T 9 74 1. During the determination, 5g laboratory samples were weighed to the nearest 0.0002g The combustion temperature was 500℃ and 50℃.
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results is not more than 0.065438 0%.
4. 10 arsenic content, measured horizontally.
Arsenic spot method according to GB /T 5009.76. When measuring, take 1.0g laboratory sample, accurate to 0.0 1g, put it in a conical flask, add 5 mL sulfuric acid and a small amount of glass beads, heat it in an adjustable electric furnace until carbonization begins, cool it, slowly add 30 (mass fraction) hydrogen peroxide until the digestive juice is clear and colorless, then heat it until white smoke appears, cool it, and carefully add/kloc-0. Take 1. 00m L arsenic (As) standard solution (equivalent to 0.00 1 gas), add 6m L sulfuric acid solution (1-}- 1), and add 35m L water to prepare limited standard solution.
4. 1 1, Determination of Fluorine in Metals
4. 1 1. 1 reagent
4. 1 1. 1 sodium sulfide solution: weigh 5g of sodium sulfide, accurate to 0.0 1g, and mix it with 10m L water and 30m L glycerol (glycerol) for dissolution. The service life of the solution is two weeks;
4. 1 1. 1.2 acetic acid solution:1-20;
4.11.1.3pb standard solution:10 t.g/mi.o.
4. 1 1.2 analysis steps
Weight 2. 0 g of laboratory sample, accurate to 0.0 0 1 g, put it in a 50 ml colorimetric tube, add 25 ml of acetone to dissolve it, add 2 ml of acetic acid solution, dilute it to 50 ml with water, add 2 drops of sodium sulfide solution, shake well, and place it in the dark for 10 minute, and the color shall not be darker than the standard colorimetric solution. The standard colorimetric solution absorbs 2.0 ml of lead (Pb) standard solution and treats it as a sample. 5. 1 Inspection is divided into factory inspection and type inspection.
5. 1. 1 Type inspection items are specified in the table 1 technical requirements. Under normal production conditions, type inspection shall be conducted at least once every two weeks. Type inspection shall also be carried out under the following circumstances.
A) update key production processes;
B) major raw materials change;
C) Stop production and resume production;
D) The result of factory inspection is quite different from that of the last type inspection;
E) stipulated in the contract.
5. 1.2 The ex-factory inspection items are ethyl benzoate content, melting point, free acid content, sulfate content and loss on drying, which should be inspected batch by batch.
5.2 Take the products in each shift as a batch number, or make a batch number after mixing in multiple shifts.
5.3 sampling shall be carried out according to GB/T 6678 and GB/T 6679. After the samples are fully mixed, they are divided into not less than 200 g by quartering method, and put into two dry and sealed sample bags respectively. The label indicates the manufacturer's name, product name, batch number or production date, sampling date and the name of the sampler. One bag is for inspection and the other bag is sealed for future reference.
5.4 The food additive ethyl benzoate shall be inspected by the quality inspection department of the production enterprise, and the production enterprise shall ensure that the ex-factory products meet the requirements of this standard. Each batch of products should be accompanied by a quality certificate in a certain format when leaving the factory, including the product name, manufacturer's name, address, batch number or production date and the serial number of this standard.
5.5 If one index in the inspection results does not meet the requirements of this standard, re-sampling shall be conducted from twice the number of packaging bags for re-inspection. Even if only one index of the reinspection results does not meet the requirements of this standard, the whole batch of products is unqualified. 6. 1 symbol
The packaging container shall be clearly marked, including the name, address, trademark, the word "food additive", product standard number, hygiene license number, batch number or production date, net quality and shelf life. There should also be signs such as "fear of rain", "fear of sun", "upward" and "limit of overlapping layers" in line with GB/T 19 1.
6.2 packaging
The food additive ethyl p-aminobenzoate acetate should be packed in polyethylene plastic bags for food, each bag has a net weight of 1k g, and every 20 bags should be a large package, or packed according to user's requirements.
6.3 Transportation and storage
The food additive ethyl p-aminobenzoate acetate should be stored in a dry, ventilated and clean warehouse. During transportation, it is not allowed to ship with harmful and toxic substances in the same car, and should be unloaded and put down gently to prevent heavy pressure, sun exposure and rain.
6.4 shelf life
Under the packaging, transportation and storage conditions that meet this standard, the shelf life of food additive ethyl paraben is three years from the date of production. Re-inspection can be carried out after the deadline, and it can still be used when the inspection results meet the requirements of this standard.