Some standard content:
ICS 71.100.01
National Standard of the People's Republic of China
GB/T4840.2—1999
o-Nitroaniline
Published on June 8, 1999
Implemented on December 1, 1999
State Administration of Quality and Technical Supervision
GB/T 4840.2—1999
The test methods in this standard are based on Japanese Industrial Standard JIS K4105:1995 "Nitroanilines". The main content and organic impurity content are determined by gas chromatography.
This standard is prepared in accordance with GB/T1.1-1993 "Guidelines for Standardization Work Unit 1: Rules for Drafting and Presentation of Standards Part 1: Basic Regulations for Standard Preparation" and GB/T1.3-1997 "Guidelines for Standardization Work Unit 1: Rules for Drafting and Presentation of Standards Part 3: Regulations for the Preparation of Product Standards". Although this standard and the Japanese Industrial Standard use the same fixed liquid phenylsiloxane OV-17, the carrier is different. The Japanese Industrial Standard is Chromosorb W-HP with a particle size of 177 to 250 μm, while this standard is Chromosorb G-AWDMCS. This standard refers to the product specifications of relevant foreign companies and the accumulated data of relevant domestic manufacturers to determine the appearance, initial melting point of dry products, content of o-nitroaniline, content of o-nitrochlorobenzene, content of p- and m-nitroaniline, content of low-boiling substances, content of high-boiling substances, and water content and other items and technical indicators.
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the National Dye Standardization Technical Committee. This standard was jointly drafted by Shenyang Chemical Industry Research Institute and Huangyan Rubber Additives (Group) Company. The main drafters of this standard are Li Chunmei and Luo Lijuan. 1
1 Scope
National Standard of the People's Republic of China
O-Nitro
o-Nitroaniline
GB/T4840.2—1999
This standard specifies the requirements, sampling, test methods, inspection rules, and marking, labeling, packaging, transportation and storage of o-nitroaniline. This standard applies to o-nitroaniline obtained by high-pressure ammonolysis, separation and filtration of o-nitrochlorobenzene. This product is mainly used in dyes, pigments, pesticides and pharmaceutical industries.
Structural formula:
Molecular formula: CHeN202
Relative molecular mass: 138.13 (according to the 1997 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB190—1990 Dangerous goods packaging mark
GB191—1990 Pictorial mark for packaging, storage and transportation
GB/T1250—1989 Methods for expressing and determining limit values GB/T2384—1992 General method for determination of melting point range of dye intermediates GB/T6682—1992 Specifications and test methods for water used in analytical laboratories (negISO3696:1987) GB/T9722—1988
General rules for gas chromatography of chemical reagents
GB/T13753—1992
3 Requirements
General method for determination of moisture content in dye intermediates
The quality of o-nitroaniline shall conform to the requirements of Table 1. Karl Fischer method and improved Karl Fischer method Table 1 Quality requirements of o-nitroaniline
Initial melting point of dry product, ℃
Purity of o-nitroaniline, %
Content of o-nitrochlorobenzene, %
Content of low-boiling substances, %
Approved by the State Administration of Quality and Technical Supervision on June 8, 1999Superior product
Qualified product
Yellow to brownish yellow crystals
1999-12- 01 Implementation
Total amount of p- and m-nitroaniline, %
Content of high boiling matter, %
Moisture content, %
4 Sampling
GB/T4840.2—1999
Table 1 (end)
Superior productsbZxz.net
Qualified products
From each batch of products (uniform products as a batch), 10% of each batch of products shall be sampled. For small batches, no less than 3 barrels shall be collected. When sampling, use a probe to collect samples including the upper, middle and lower parts. The total amount of sampling shall not be less than 200g. After grinding and mixing the samples, they shall be divided into two clean and dry wide-mouth bottles with ground stoppers. Labels shall be pasted on the bottles, indicating: manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection, and the other bottle is sealed with paraffin and kept for future reference. 5 Test methods
Unless otherwise specified, the reagents used in this standard are analytically pure reagents, and water should meet the specifications of Grade 3 water in GB/T6682. The test results are determined by the rounded value comparison method in GB/T1250. 5.1 Appearance
The appearance is determined by visual inspection.
5.2 Determination of initial melting point of dry product
According to the provisions of GB/T2384, the sample must be dried at 45-50℃ for 30min in an infrared oven or under an infrared lamp. The difference between the results of two parallel determinations is not greater than 0.2℃, and the arithmetic mean is taken as the determination result. 5.3 Determination of o-nitroaniline content and its organic impurity content 5.3.1 Summary of methods
Gas chromatography is used to separate o-nitroaniline and organic impurity components on a packed gas chromatographic column, and the peak area normalization method is used for quantification after detection by hydrogen flame ionization detector (FID). 5.3.2 Instruments and Devices
Gas chromatograph: The sensitivity and stability of the instrument shall comply with the provisions of GB/T9722; Detector: Hydrogen flame ionization detector FID; Data processor: Recorder with full scale of 10mV and response time of 1s or data processor with this function; Chromatographic column: Glass column or stainless steel column with inner diameter of 3.2~3.5mm and length of 2m; Micro-injection syringe: 10μL.
5.3.3 Preparation of Chromatographic Column
5.3.3.1 Filler
Carrier: Chromosorb G-AWDMCS177~250μm (80~60 mesh), stationary liquid: phenylsiloxane 0V-17 (maximum operating temperature 300℃); Solvent: chloroform;
Coating degree: stationary liquid/carrier = 4/100.
5.3.3.2 Coating of the fixing solution
Weigh 0.8g of 0V-17 in a 100mL beaker, then add chloroform equivalent to the volume of 20g of the carrier. After the 0V-17 is completely dissolved, slowly pour in 20g of the carrier to make it completely soaked (about 10 minutes). Place the beaker in a fume hood and under an infrared lamp, allow the solvent to evaporate slowly until dry (the beaker should be tapped frequently to ensure uniform coating). Then move to a 90100℃ oven and dry for about 30 minutes, then take out for use. 5.3.3.3 Filling of stationary phase
GB/T4840.2—1999
Plug glass wool into one end of the chromatographic column connected to the detector, wrap it with gauze, connect it to a vacuum pump, connect the other end to a funnel, slowly pour in the dried stationary phase under vacuum, tap the chromatographic column gently to make the filling even and tight, and continue tapping for 5-10 minutes after filling, plug the filled chromatographic column with glass wool, and prepare for aging.
5.3.3.4 Aging of chromatographic column
Install the filled chromatographic column into the column box of the chromatograph, do not connect the detector after the column, pass nitrogen at a flow rate of 5-10mL/min, and age at 270℃ for 8-10h.
5.3.4 Chromatographic conditions (optimal operating conditions can be selected according to different instruments) Column temperature: 220℃
Vaporization temperature: 250℃,
Detection temperature: 250℃;
Carrier gas flow rate (N2): 50mL/min,
Combustion gas flow rate (H2): 50mL/min;
Auxiliary gas flow rate (O2): 500mL/min; Paper speed: 3mm/min;
Injection volume: 2~3μL,
Quantitative method: Peak area normalization method ;
Resolution: ≥1.0
5.3.5 Preparation of standard stock solution and determination of correction factor 5.3.5.1 Reagents
Ethyl acetate;
O-nitroaniline: purity ≥99.5%;
P-nitroaniline: refined product (recrystallized from ethanol three times until no impurities are detected under the test conditions);M-nitroaniline: refined product (recrystallized from ethanol three times until no impurities are detected under the test conditions);O-nitrochlorobenzene: refined product (recrystallized from ethanol three times until no impurities are detected under the test conditions);5.3.5.2 Preparation of standard stock solution
According to the requirements of Table 2, accurately weigh various reagents (accurate to 0.0002g) into a clean and dry volumetric flask, dissolve with ethyl acetate, and dilute to the mark. The shelf life of the standard stock solution is three months. Table 2 Preparation of standard stock solution
Reagent name
Weighing amount g
Volume after dilution, mL
o-Nitrochlorobenzene
5.3.5.3 Preparation of standard mixed solution
p-Nitroaniline
m-Nitroaniline
o-Nitroaniline
In five numbered 10mL brown volumetric flasks, prepare mixed solutions No. 1, 2, 3, 4, and 5 according to Table 3. The shelf life of the standard mixed solution is one month.
Preparation of standard mixed solution
Single standard solution
Liquid A (o-nitrochlorobenzene), mL
Liquid B (p-nitroaniline), mL
Single standard solution
Liquid C (m-nitroaniline), mL
Single standard solution
Liquid D (o-nitroaniline), mL
Dilute with ethyl acetate to total volume, mL
5.3.5.4 Determination and calculation of correction factor
GB/T4840.2—1999
Table 3 (end)
Under the selected chromatographic conditions, add 2μL of the standard mixed solution respectively. After the peaks of each component are eluted, calculate the correction factors of o-nitrochlorobenzene, p-nitroaniline and m-nitroaniline respectively. The peak before o-nitrochlorobenzene is a low-boiling product, and the correction factor is calculated based on o-nitrochlorobenzene; the peak after p-nitroaniline is a high-boiling product, and the correction factor is calculated based on p-nitroaniline. The correction factor of each component is calculated according to formula (1):
W—mass of o-nitroaniline, g,
The chromatogram is shown in Figure 1.
.........(1)
25 nin
1Solvent;2—Low boiling substance;3—o-nitrochlorobenzene;4—o-nitroaniline;5—m-nitroaniline;6—p-nitroaniline;7—High boiling substance Gas chromatogram of o-nitroaniline
5.3.6Analysis steps
Weigh 1 g (accurate to 0.01 g) of o-nitroaniline sample into a 10 mL brown volumetric flask and dilute to the mark with ethyl acetate. Inject 2-3 μL of sample under the selected conditions. After all components have finished emitting peaks, calculate the percentage of each component 4
according to the peak area and relative correction factor of each component according to formula (2):
GB/T4840.2-1999
5×(100-W）
E(f:·A)
W——water content, %. The difference between the two parallel determination results of purity is not more than 0.2%, and the difference between the two parallel determination results of each organic impurity content is not more than 0.05%. Take their arithmetic mean as the determination result. 5.4 Determination of moisture content
According to the provisions of GB/T13753, the solvent is chloroform + methanol = 3 + 1 (V1 + V2), and the sample is 0.5g. 6 Inspection rules
6.1 Inspection classification
All items specified in the table are factory inspection items 6.2 Factory inspection
O-nitroaniline should be inspected by the quality inspection department of the manufacturer according to the requirements of this standard. The manufacturer should ensure that all products shipped meet the requirements of this standard. Each batch of products shipped should be accompanied by a quality certificate in a certain format. 6.3 User acceptance
The user unit has the right to inspect the received o-nitroaniline in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
6.4 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 7 Marking, labeling, packaging, transportation and storage 7.1 Marking
O-nitroaniline packaging barrels should have clear markings, indicating the manufacturer's name, address, product name, trademark, batch number, grade, gross weight, net weight and production date, and the word "toxic" and diagram according to the requirements of GB190 and GB191. 7.2 Labeling
Each batch of packaged products should be accompanied by a label of a certain format, which includes: manufacturer's name, address, product name, batch number, grade, net weight, production date, proof that the product quality meets the requirements of this standard and the number of this standard. 7.3 Packaging
O-nitroaniline is packaged in woven bags or iron drums lined with plastic bags (plastic bags must be tied), with a net weight of 25kg per bag (barrel). If the user needs other packaging, it can be determined through negotiation.
7.4 Transportation
It should be protected from exposure, collision and rain during transportation. 7.5 Storage
The product should be stored in a cool, dry and ventilated warehouse.2 Inspection by the manufacturer
O-nitroaniline shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. 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 certificate in a certain format. 6.3 User acceptance
The user unit has the right to inspect the received o-nitroaniline in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
6.4 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 7 Marking, labeling, packaging, transportation and storage 7.1 Marking
O-nitroaniline packaging barrels should have clear markings, indicating the manufacturer's name, address, product name, trademark, batch number, grade, gross weight, net weight and production date, and the word "toxic" and diagram according to the requirements of GB190 and GB191. 7.2 Labeling
Each batch of packaged products should be accompanied by a label of a certain format, which includes: manufacturer's name, address, product name, batch number, grade, net weight, production date, proof that the product quality meets the requirements of this standard and the number of this standard. 7.3 Packaging
O-nitroaniline is packaged in woven bags or iron drums lined with plastic bags (plastic bags must be tied), with a net weight of 25kg per bag (barrel). If the user needs other packaging, it can be determined through negotiation.
7.4 Transportation
It should be protected from exposure, collision and rain during transportation. 7.5 Storage
The product should be stored in a cool, dry and ventilated warehouse.2 Inspection by the manufacturer
O-nitroaniline shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. 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 certificate in a certain format. 6.3 User acceptance
The user unit has the right to inspect the received o-nitroaniline in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
6.4 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 7 Marking, labeling, packaging, transportation and storage 7.1 Marking
O-nitroaniline packaging barrels should have clear markings, indicating the manufacturer's name, address, product name, trademark, batch number, grade, gross weight, net weight and production date, and the word "toxic" and diagram according to the requirements of GB190 and GB191. 7.2 Labeling
Each batch of packaged products should be accompanied by a label of a certain format, which includes: manufacturer's name, address, product name, batch number, grade, net weight, production date, proof that the product quality meets the requirements of this standard and the number of this standard. 7.3 Packaging
O-nitroaniline is packaged in woven bags or iron drums lined with plastic bags (plastic bags must be tied), with a net weight of 25kg per bag (barrel). If the user needs other packaging, it can be determined through negotiation.
7.4 Transportation
It should be protected from exposure, collision and rain during transportation. 7.5 Storage
The product should be stored in a cool, dry and ventilated warehouse.
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