Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2078—91
2-Cyano-4-nitroaniline
Published on July 17, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1992
Chemical Industry Standard of the People's Republic of China
2-Cyano-4-nitroaniline
Subject Content and Scope of Application
HG2078—91
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for 2-cyano-4-nitroaniline.
This standard applies to 2-cyano-4-nitroaniline prepared from o-chlorotoluene by ammoxidation, nitration and amination. This product is mainly used as a dye intermediate.
Structural formula:
Molecular formula: CH0,Ns
Relative molecular mass: 163.13 (according to the international relative atomic mass in 1987) 2 Reference standards
Dangerous goods packaging mark
GB191 Pictorial mark for packaging storage
GB/T2384 General method for determination of melting point range of dye intermediates GB2386 Method for determination of moisture content of dyes and dye intermediates 3 General rules for sampling of chemical products
GB6678
3 Technical requirements
The quality of 2-cyano-4-nitroaniline shall meet the requirements of the following table: Index
2-cyano-4-nitroaniline content, %
Initial melting point of dry product, ℃
Water content, %
Test method
4.1 Appearance
Determine by visual method.
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 17, 1991. Superior product
Light yellow powder
Qualified product
Implemented on January 1, 1992
4.2 Determination of 2-cyano-4-nitroaniline content 4.2.1 Method summary
HG2078--91
2-cyano-4-nitroaniline was subjected to reverse phase chromatography, with methanol-water as the mobile phase and ODS-C18 as the stationary phase. The content was calculated by the internal standard peak area method, with 2,4-dinitroaniline as the internal standard. 4.2.2 Reagents and solutionswwW.bzxz.Net
4.2.2.1 Anhydrous ethanol (GB678);
4.2.2.2 Methanol (GB683);
4.2.2.3 N,N-dimethylformamide;
4.2.2.4 2-cyano-4-nitroaniline standard: content ≥99.7%; 4.2.2.5 2,4-nitroaniline standard: content ≥99.7%. 4.2.3 Instruments and chromatographic conditions
Liquid chromatograph;
Infusion pump: flow range 0.1～5mL/min; flow stability ±2%; maximum usable pressure 2×10°Pa; chromatographic column: stainless steel column with an inner diameter of 4.6mm and a length of 150mm; stationary phase: wet-filled 5umODSC18 or other brands of bonded stationary phases with the same performance; detector: UV wavelength 300nmD lamp.
Recorder: 10mV recorder or general chromatography data processor with the same performance; Micro syringe: Use 10uL micro syringe for the column head. When using a quantitative valve, use a flat-head syringe of corresponding capacity; Sensitivity: 0D, 0.08;
Mobile phase ratio: methanol + water = 2 + 1;
Flow rate: 1mL/min;
Injection volume: 3uL.
4.2.4 Preparation of standard solution and determination of correction factor Weigh 0.05g (accurate to 0.0002g) of refined 2-cyano-4-nitroaniline standard into 12 25mL volumetric flasks, and then add 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09g of 2,4-dinitroaniline standard in turn, and dissolve each with 1mL of N,N-dimethylformamide. After complete dissolution, dilute to the mark with ethanol and shake well. Take 3uL of each with a micro syringe and inject into the injection valve. Press the "Start" key, and under the given chromatographic program, the chromatographic processor prints out the peak area, and draws a standard curve with the weight ratio of 2,4-dinitroaniline to 2-cyano-4-nitroaniline as the horizontal axis and the peak area ratio of 2,4-dinitroaniline to 2-cyano-4-nitroaniline as the vertical axis.
The correction factor of 2-cyano-4-nitroaniline is calculated according to formula (1): A.Xm
Where: f: —2-cyano-4-nitroaniline correction factor; A2,4-dinitroaniline standard peak area, mm; m: —2-cyano-4-nitroaniline mass, g; A —2-cyano-4-nitroaniline peak area, mmm——2,4-dinitroaniline standard mass, g. 4.2.5 Determination of 2-cyano-4-nitroaniline content (1)
Weigh 0.05g of sample (accurate to 0.0002g) and 0.05g of 2,4-dinitroaniline (accurate to 0.0002g) into a 25mL volumetric flask and dissolve in 1mL of N,N-dimethylformamide. After complete dissolution, dilute to scale with ethanol and inject 3uL according to the chromatographic conditions. The chromatographic processor prints out the peak area and calculates the analysis results using formula (2). The chromatogram is shown in Figure 1. The 2-cyano-4-nitroaniline content is calculated using formula (2): fA.·m×100%
Where: f—2-cyano-4-nitroaniline correction factor HG2078-91
A—2-cyano-4-nitroaniline peak area, mm2; m. —Mass of 2,4-dinitroaniline standard, g; As——peak area of 2,4-dinitroaniline standard, mm2; m
Mass of a sample,.
The difference between the results of two parallel determinations shall not be greater than 1%, and the arithmetic mean shall be taken as the determination result. 2
Shelf life, ml
Chromatogram of 2-cyano-4-nitroaniline
1—Solvent peak; 2—2-cyano-4-nitroaniline; 3—2,4-dinitroaniline; 4—Unknown substance 4.3 Initial melting point of dry product
According to the provisions of GB2384, the sample is dried at 100-105℃ for 1h. 4.4 Water
According to the method specified in Chapter 2 of GB2386. 5 Inspection rules
5.12-Cyano-4-nitroaniline shall be inspected by the inspection department of the manufacturer. The manufacturer shall ensure that all 2-cyano-4-nitroaniline shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 The user has the right to inspect whether the received 2-cyano-4-nitroaniline meets the requirements of this standard in accordance with the requirements of this standard. 5.3 Take the uniform products in each package as a batch, and take samples from 10% of the packaging barrels of each batch of products. The small batch sampling shall not be less than 3 barrels. When sampling, use a probe to take samples from the upper, middle and lower parts of the opened barrel. The sampling volume shall not be less than 500g. 5.4 After the samples are evenly mixed, they are placed in two clean, dry wide-mouth bottles with ground stoppers and sealed with paraffin. Labels are attached to indicate the product name, manufacturer name, grade, batch number and sampling date. One bottle is inspected by the inspection department and the other bottle is kept for reference. 5.5 If any index of the test result does not meet the requirements of this standard, a sample should be taken from the twice amount of packaging for retest. If even one item of the retest result does not meet the requirements of this standard, the whole batch of products cannot be accepted. 3
HG207891
5.6 When the supply and demand parties have disputes over the quality of the product, arbitration inspection should be carried out according to the test methods specified in this standard. 6 Marking, packaging, transportation and purchase and storage
6.1 The packaging barrel should be painted with a firm mark. The content includes: manufacturer name, product name, grade, batch number, net weight, tare weight, trademark, this standard number and proof that the product meets the requirements of this standard. 6.2 2-Cyano-4-nitroaniline is packed in an iron barrel lined with a plastic bag. The net weight of each barrel is 25kg, 50kg, and 100kg. 6.3 2-Cyano-4-nitroaniline should be handled with care and should not come into contact with the skin to prevent inhalation. The container should be airtight, and should not be exposed to sunlight or moisture. It should be stored in a cool, ventilated and dry place. A12-Cyano-4-nitroaniline standard preparation HG2078-91
Appendix A
Preparation of standard
(Supplement)
Weigh 5g of 2-cyano-4-nitroaniline sample on a balance and put it in a 400mL beaker. Add 200mL of ethanol to a 70℃ constant temperature water bath and stir continuously to dissolve it. After it is completely dissolved, vacuum filter and discard the residue. Cool the filtrate to -5~0℃ in an ice bath, recrystallize it, and vacuum filter it. Repeat this process several times, dry it in an oven at 100105℃ for 1h, and analyze it with a liquid chromatograph. The content was measured by the normalization method to be 99.7%, which is regarded as a standard.
2,Preparation of 4-dinitroaniline standard
Weigh 5g of 2,4-dinitroaniline sample on a balance and place it in a 400mL beaker. Add 200mL of ethanol and place it in a 70℃ constant temperature water bath. Stir continuously to dissolve it. After it is completely dissolved, vacuum filter and discard the residue. Cool the filtrate in an ice bath to -5~0℃, recondense it and vacuum filter it. Repeat this process several times. The sample is dried in an oven at 100~105℃ for 1h and analyzed by liquid chromatography. The content measured by the normalization method is ≥99.7%, which is regarded as a standard.
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 jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Hunan Xiangtan Dyestuff Chemical General Factory and the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Liu Penglan, He Fanghui, Wang Qiongxuan, He Jian, and Song Qinghu. 5
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