HG/T 2306-1992 Industrial 1-phenyl-3-methyl-5-pyrazolone HG/T2306-1992 Standard download decompression password: www.bzxz.net

Chemical Industry Standard of the People's Republic of China
HG2306-92
Industrial 1-phenyl-3-methyl-5-pyrazolone
Published on May 17, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993
W Chemical Industry Standard of the People's Republic of China
Industrial 1-phenyl-3-methyl-5-pyrazolone
1 Subject Content and Scope of Application
HG2306-92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation, compensation and storage of industrial 1-phenyl-3-methyl-5-pyrazolone (also known as pyrazolone).
This standard applies to 1-phenyl-3-methyl-5-pyrazolone prepared by the diketene method. This product is mainly used in pharmaceutical dyes and other industries. Molecular formula: CoH1oON2
Structural formula:
Relative molecular mass: 174.20 (according to the international relative atomic mass in 1989) 2 Reference standards
GB601 Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in chemical reagent test methods GB603
GB617 Chemical trial production General method for determination of melting point range GB1250
Expression and determination method of limit values ​​GB6284
GB6678
GB6679
GB8170
3 Technical requirements
General method for determination of water content in chemical products Gravimetric method
General rules for sampling of chemical products
General rules for sampling of solid chemical products
Rules for rounding off values
3.1 Appearance: light yellow crystals or powder.
3.2 Industrial 1-phenyl-3-methyl-5-pyrazolone should meet the requirements of the following table: Approved by the Ministry of Chemical Industry of the People's Republic of China on May 17, 1992 and implemented on January 1, 1993
W Pyrazolone content, %
Melting point range, ℃
Heating loss, %
Solubility in 5% hydrochloric acid
4 Test method
HG2306-92
First-class product
127~129
Qualified product
127~130
Unless otherwise specified, the reagents and water used in this test method are analytical reagents and distilled water or water of equivalent purity. The standard titration solutions and preparations used in this test method are prepared according to GB601 and GB603 unless otherwise specified. 4.1 Determination of content
4.1.1 Principle of the method
1-phenyl-3-methyl-5-pyrazolone in the sample undergoes nitrosation reaction with sodium nitrite standard titration solution under acidic conditions, and the starch potassium iodide indicator indicates the end point.
4.1.2 Reagents and solutions
4.1.2.1 Hydrochloric acid solution: 1+1(V+V); 4.1.2.2 Standard sodium nitrite titration solution: c(NaNO)=0.1mol/L. 4.1.2.3 Starch potassium iodide indicator solution, 5g/L, take 0.5g starch, add 5mL cold water, stir well, then slowly pour into 100mL boiling distilled water, stir and boil, cool to room temperature, take 100mL of the upper layer liquid, add 0.5g potassium iodide, and dissolve to obtain. This solution should be freshly prepared and replaced after 24h.
4.1.3 Instruments
General laboratory instruments.
4.1.4 Analysis stepsWww.bzxZ.net
Weigh 0.3~0.4g of the ground sample, accurate to 0.0002g, and place it in a dry 250mL beaker. Add 15mL of hydrochloric acid solution (4.1.2.1). After it is completely dissolved, add 100mL of distilled water. Insert the tip of the burette injected with 0.1mol/L sodium nitrite standard titration solution to about 2/3 below the liquid surface, control the solution temperature at 10~15℃ and slowly titrate, stirring as you drop. When it is 12mL away from the end point, lift the tip of the burette out of the liquid surface, wash the tip with a small amount of water, and continue to titrate slowly until a thin glass rod is dipped in a small amount of solution and rubbed across a white porcelain plate with starch potassium iodide indicator solution. It immediately turns blue. Stir for another 3 minutes. If it still turns blue when tested with a glass rod, it is the end point. At the same time, do a blank test.
4.1.5 Calculation of results
The content X of industrial 1-phenyl-3-methyl-5-pyrazolone expressed as mass percentage is calculated according to the following formula: c(V -V) × 0. 174 2 × 100
Wherein: c——actual concentration of sodium nitrite standard titration solution, mol/L; V——volume of sodium nitrite standard titration solution consumed by the sample, mL; V.——volume of sodium nitrite standard titration solution consumed by the blank, mL; m
——mass of the sample, g;
0.1742——mass of 1-phenyl-3-methyl-5-pyrazolone equivalent to 1.00mL sodium nitrite standard titration solution [c(NaNO2)=1.000mol/L], expressed in grams. 2
W.bzsoso.coIHG2306—92
Determination results: Take the arithmetic mean of two parallel determinations as the result. 4.1.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.3%. 4.2 Determination of melting point range
4.2.1 Determination method
Take the sample after the "heating loss" determination and carry out in accordance with the provisions of GB617. 4.2.2 Allowable difference
The difference between the results of two parallel determinations, the initial melting point and the final melting point shall not exceed 0.2℃. Take the arithmetic mean of two parallel determinations as the determination result. 4.3 Determination of heating loss
Carry out in accordance with the provisions of GB6284.
4.3.1 Drying temperature: 80±2℃.
4.3.2 Weigh the sample amount: 5~10g.
4.3.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.05%. 4.4 Solubility test in 5% hydrochloric acid
4.4.1 Reagents and solutions
Hydrochloric acid solution: 5%.
4.4.2 Analysis steps
Weigh 1.0g of the sample, accurate to 0.01g, put it into a 100mL beaker, add 50mL of 5% hydrochloric acid solution, heat to 7080℃ to dissolve, and immediately observe the dissolution properties of the solution. 4.4.3 Result indication
The solution is completely dissolved and is a first-class product.
5 Inspection rules
5.1 Industrial 1-phenyl-3-methyl-5-pyrazolone should be inspected by the quality inspection department of the manufacturer, and the manufacturer should ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory should be accompanied by a quality certificate in a certain format. The content includes: manufacturer name, product name, batch number, production date, product quality and this standard number. 5.2 Industrial 1-phenyl-3-methyl-5-pyrazolone is a uniform product, not more than 5 tons per batch. 5.3 The sampling method for industrial 1-phenyl-3-methyl-5-pyrazolone shall be carried out in accordance with GB6678 and GB6679. The sampling volume shall not be less than 300g. 5.4 The samples taken shall be carefully mixed and divided into two clean and dry brown bottles with ground stoppers. Labels shall be affixed to the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and analysis, and the other bottle is sealed and kept for three months. For inspection. 5.5 The user has the right to verify the quality of the industrial 1-phenyl-3-methyl-5-pyrazolone products received in accordance with the inspection rules and test methods specified in this standard to verify whether its quality meets the requirements of this standard. 5.6 When inspecting the product, if it is found that one of the indicators in the inspection results does not meet the requirements of this standard, samples should be taken from twice the number of packaging units for re-inspection. If even one of the indicators in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.7 The judgment of the inspection results shall be carried out according to the "rounded value comparison method" in GB1250, and the rounding shall be carried out according to the provisions of GB8170. 5.8 When the supply and demand parties have a dispute over the quality of the product, the supply and demand parties shall jointly agree on arbitration. 6 Marking, packaging, transportation, storage
6.1 The packaging bags of industrial 1-phenyl-3-methyl-5-pyrazolone products should be painted with a firm mark, which includes: manufacturer name, product name, trademark, this standard number, production date, batch number and net weight, and the words "do not get wet" should be marked. 6.2 Industrial 1-phenyl-3-methyl-5-pyrazolone should be packed in plastic woven bags lined with plastic bags, with a net weight of 25kg per bag. 6.3 Industrial 1-phenyl-3-methyl-5-pyrazolone products should be transported in vehicles or vessels with canopies. If there is no canopy, it should be covered with canvas. It is required to be loaded and unloaded gently during transportation.
6.4 Industrial 1-phenyl-3-methyl-5-pyrazolone products should be stored in a ventilated and dry place to prevent moisture and heat, and should not be stacked with flammable items.
Additional Notes:
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 Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nantong Acetic Acid Chemical Plant. The main drafters of this standard are Chen Zhuying, He Xunmei, and Zhou Lixian. This standard refers to the Soviet national standard OCT9593-74 (86) "Industrial 1-phenyl-3-methyl-5-pyrazolone". From the date of implementation of this standard, the former standard HG2-387-66 "Pyrazolone" issued by the Ministry of Chemical Industry of the People's Republic of China will be invalid. W.
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