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Chemical Industry Standard of the People's Republic of China
HG2278-92
Acetoacetanilide
1992-06-01 Issued
Ministry of Chemical Industry of the People's Republic of China
1993-01-01 Implementation
Chemical Industry Standard of the People's Republic of China
First Acetanilide
1 Subject Content and Scope of Application
HG2278-92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage requirements of acetoacetanilide products.
This standard applies to acetoacetanilide prepared by the condensation of diketene and aniline. Molecular formula: CioHuoON
Structural formula:
NHCOKHCOCH
Relative molecular mass: 177.20 (according to the international relative atomic mass in 1989) 2 Reference standards
Preparation of standard solution for titration analysis (volumetric analysis) Chemical reagents
GB603 Preparation of preparations and products used in chemical reagent test methods Methods for expressing and determining limit values GB1250
GB/T2384 General method for determination of melting point range of dye intermediates Technical requirements
The quality of acetoacetanilide shall comply with the requirements of Table 1. Table 1
(1) Appearance
(2) Initial melting point of dry product, ℃
(3) Content (total nitrite value), %
(4) Volatile matter content, %
(5) Alkali solubility turbidity
Test method
4.1 Appearance
Determine by visual method.
2 Determination of initial melting point of dry product
Approved as superior product by the Ministry of Chemical Industry of the People's Republic of China on June 1, 1992
White to light yellow crystalline powder or
Flake crystals
Clear and transparent
White to light yellow or very light pink
Colored powder or flake products
Basically clear and transparent
Implemented on January 1, 1993
HG2278-92
Performed in accordance with the provisions of GB2384. The sample is dried at 60-65℃ to constant weight. 4.3 Determination of content (total nitrosation value)
4.3.1 Principle
Aromatic amine acylates are quantitatively nitrosated with sodium nitrite in the presence of inorganic acid, and the excess sodium nitrite is detected by iodide ion to determine the end point.
4.3.2 Reagents and solutions
4.3.2.1 Glacial acetic acid (GB676);
4.3.2.2 Hydrochloric acid (GB622);
4.3.2.3 Sodium hydroxide (GB629): 40g/L solution; 4.3.2.4 Sodium nitrite (GB633): c (NaNO2) = 0.5mol/L standard titration solution, prepared and calibrated according to the method specified in Article 4.22 of GB601, and starch-potassium iodide test paper is used to judge the end point. 4.3.2.5 Starch-potassium iodide test paper: prepared according to the method specified in Article 4.2.3 of GB603. 4.3.3 Analysis steps
Weigh about 1.2g of the sample (accurate to 0.0002g) in a 400mL beaker, add 8mL of sodium hydroxide solution (4.3.2.3) and 150mL of water to dissolve at 25-35℃, add 100mL of glacial acetic acid (4.3.2.1) and 25mL of hydrochloric acid (4.3.2.2) under constant stirring, add water to a total of about 300mL, titrate with sodium nitrite standard titration solution (4.3.2.4), insert the tip of the burette about 10mm below the solution during titration, slowly add sodium nitrite standard titration solution at 10℃ and stirring, keep 1015℃, when approaching the end point, lift the tip of the burette from the liquid surface and add drop by drop, dip a drop of the test solution with a glass rod on the starch-potassium iodide test paper and it will show a slight blue color, and the test paper will still show a slight blue color after 5 minutes, which is the end point. Under the same conditions, do a blank test. 4.3.4 Calculation of results
The mass percentage of the total nitrite value (X) is calculated according to formula (1): Xi = (V1-V2)X0.177 2bzxZ.net
Wherein: c-
-actual concentration of sodium nitrite standard titration solution, mol/L: X100
Vi--volume of sodium nitrite standard titration solution consumed by titrating the sample, mL, V2--volume of sodium nitrite standard titration solution consumed by blank test, mL; (1
0.1772--mass of acetoacetanilide equivalent to 1.00mL sodium nitrite standard titration solution [c(NaNO,)=1.000mol/L], expressed in grams;
m1--mass of sample, g.
4.3.5 Allowable difference
The difference between two parallel determination results shall not exceed 0.3%. The arithmetic mean of the parallel determination results shall be taken as the determination result. 4.4 Determination of volatile content
4.4.1 Principle
Place the sample in a vacuum desiccator and remove the volatiles until constant weight is reached. Calculate the volatile content based on the weight of the sample and the weight of the sample after constant weight.
4.4.2 Instrument
Vacuum desiccator:
Vacuum pump: 30L rotary vane type.
4.4.3 Analysis steps
Weigh about 2g of the sample (accurate to 0.0002g) into a weighing bottle that has been weighed to a constant weight, move the weighing bottle and the sample into the vacuum desiccator, turn on the vacuum pump, and vacuum dry at 4000Pa until constant weight is reached (about 3h). 4.4.4 Calculation of results
The mass percentage of volatile matter (X2) is calculated according to formula (2): 2||tt ||Where: m2——mass of the sample, g;
HG2278—-92
m2-msx100.
m3——mass of the sample after vacuum drying and constant weight, g. 4.4.5 Allowable difference
The difference between two parallel determination results shall not exceed 0.03%. The arithmetic mean of the parallel determination results shall be taken as the determination result. 4.5 Alkali solubility turbidity
4.5.1 Principle
After the sample is dissolved in sodium hydroxide solution, it is compared with the silver chloride turbidity standard solution to determine the alkali solubility turbidity of the sample. 4.5.2 Instrument
Colorimetric tube: A set of 25mL stoppered standard colorimetric tubes, which are required to be equal in diameter, height and wall thickness. 4.5.3 Reagents and solutions
4.5.3.1 Sodium chloride (GB1266)
4.5.3.2 Sodium hydroxide (GB629) solution: 10g/L4.5.3.3 Nitric acid (GB337): (1+3) solution4.5.3.4 Silver nitrate (GB670) standard solution: c(AgNO) = 0.1mol/L, prepared according to the method specified in GB601. 4.5.4 Preparation of silver chloride turbidity standard solution: (2)
4.5.4.1 Preparation of No. 1 chlorine standard solution Weigh 0.164g (accurate to 0.0002g) of sodium chloride (4.5.3.1) burned to constant weight at 500~600℃ in a 1000mL volumetric flask, add water to dissolve, and dilute to the mark with water, shake well and set aside. This solution contains 0.1mg chlorine in 1mL. 4.5.4.2 Preparation of No. 2 chlorine standard solution Dilute No. 1 chlorine standard solution with water 10 times. This solution contains 0.01 mg chlorine per mL. 4.5.4.3 Preparation of No. 3 chlorine standard solution Dilute No. 1 chlorine standard solution with water 100 times. This solution contains 0.001 mg chlorine per mL. 4.5.5 Preparation of turbidity standard solution:
Prepare turbidity standard solutions in 5 colorimetric tubes according to Table 2, cover the colorimetric tube stoppers, shake well, and leave for 15 minutes. Table 2 Turbidity standard solution
Clear and transparent
Basically clear and transparent
Slightly turbid
4.5.6 Analysis steps
Chlorine standard solution, mL
Turbidity standard
Water, mL
Nitric acid, mL
Silver nitrate solution (number of drops)
Weigh about 2g of the sample (accurate to 0.0002g) in a 100mL beaker, add 50mL of sodium hydroxide (4.5.3.2) solution and dissolve at 25~30℃, wait until it cools to room temperature, and measure 20mL of the solution into a colorimetric tube. Place the colorimetric tube containing the sample solution and the turbidity standard solution on the colorimetric tube rack, and use black paper to contrast the bottom of the colorimetric tube, facing the white background, and observe from top to bottom. The corresponding turbidity grade is obtained by colorimetric comparison of the axis. 5 Inspection rules
5.1 Inspection categories
All items specified in Table 1 are factory inspection items. 5.2 Sampling method
Random sampling is carried out in batches. The manufacturer considers the uniform products mixed once as a batch, while the user considers the products with the same batch number 3
HG2278-92
received from the same manufacturer as a batch. The number of samples shall not be less than VCN, which is the number of bags (barrels) of each batch of products. 》If there is a decimal, it shall be rounded up to an integer. When sampling small batches of products, the number of samples shall not be less than 3 bags (barrels). When sampling, use a sampler to take samples from the upper, middle and lower parts respectively. After mixing evenly, take about 200g and divide them into two clean and dry ground-mouth brown bottles. The bottle mouths are sealed with paraffin and labeled with the manufacturer's name, batch number and sampling time. One bottle is for inspection and the other is for storage for future reference. 5.3 Production inspection
Acetoacetanilide should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all acetoacetanilide shipped out of the factory meets the requirements of this standard and is accompanied by a quality certificate in a certain format. The test results shall be determined according to the rounded value comparison method in GB1250. 5.4 User Acceptance
The user has the right to verify the acetoacetanilide received in accordance with the provisions of this standard. Verify whether its quality meets the requirements of this standard.
5.5 Re-test
If the test results do not meet the requirements of this standard, samples shall be taken from twice the amount of woven bags (barrels) for re-testing. Even if only one indicator fails in the re-test results, the entire batch of products shall be unqualified. 5.6 Arbitration
If the supply and demand parties have disputes over the results and need arbitration, the arbitration institution may be selected by negotiation between the two parties, and the arbitration method shall be carried out in accordance with the provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 The woven bag (barrel) should have a firm and clear mark, indicating the manufacturer's name, product name, registered trademark, standard number, batch number, specification, gross weight, net weight, and attached with a product quality certificate. 6.2 Acetoacetanilide should be packed in a woven bag (barrel) lined with a plastic bag, with a net weight of 25kg per bag (barrel). Other packaging should be negotiated with the user.
6.3 Handle with care during transportation, prevent fire, sun and rain, and do not damage the packaging. 6.4 The product should be stored in a cool, dry and ventilated warehouse. Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Qingdao Dyestuff Factory. The main drafters of this standard are Tao Meixin and Wen Huiqiong. This standard refers to the Japanese Industrial Standard JISK4173-81 "Acetoacetanilide". 4
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