Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2669-95
O-aminoanisole
Published on April 5, 1995
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1996
W Chemical Industry Standard of the People's Republic of China
O-hydrogenanisole
Subject Content and Scope of Application
HG/T2669-95
Replaces GB10659-89
This standard specifies the technical requirements, test methods, inspection rules, and requirements for marking, packaging, transportation and storage of o-aminoanisole.
This standard applies to o-aminoanisole obtained by reduction of o-nitroanisole. This product is mainly used in dyes, fragrances and pharmaceutical intermediates.
Molecular formula: C,H.NO
Structural formula:
Relative molecular mass: 123.15 (according to the international relative atomic mass in 1991) 2 Reference standards
GB/T2385
GB/T9722
General method for determination of crystallization point of dye intermediates General rules for gas chromatography of chemical reagents
GB/T13753 General method for determination of moisture content of dye intermediates Karl Fischer method and modified Karl Fischer method. 3 Technical requirements
O-aminoanisole shall meet the requirements of Table 1.
Crystallization point, ℃
o-Anisole, %
Low boiling substance, %
o-Chloroaniline, %
p-Anisole, %
High boiling substance, %
Water, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995. Superior product
Qualified product
Yellow-brown to dark brown transparent liquid
Implemented on January 1, 1996
.bzsoso, cOn4 Test method
4.1 Determination of appearance
Determine by visual method.
4.2 Determination of crystallization point
HG/T2669—95
Take 50mL of o-aminoanisole sample in a 125mL wide-mouth bottle, add 25g of 4A molecular sieve, cover the bottle cap and dehydrate for 30min (shake 3-4 times during this period), and then proceed according to the relevant provisions of GB/T2385. During the test, when the sample is cooled to below -2℃, add a small amount of seed crystals with a glass rod (add a small amount of dried o-aminoanisole sample to a test tube, cool to -2℃, add a small amount of p-aminoanisole crystals, stir with a glass rod until all crystals are precipitated, and use this as seed crystals). 4.3 Determination of o-aminoanisole, o-chloroaniline, p-aminoanisole, low-boiling and high-boiling substances. 4.3.1 Summary of methods
Gas chromatography is used for determination, and area normalization method is used for quantification. 4.3.2 Instruments
4.3.2.1 Gas chromatograph: should comply with the provisions of Chapter 5 of GB/T97224.3.2.2 Detector: hydrogen flame ionization detector;4.3.2.3 Chromatographic column: stainless steel column or glass column with an inner diameter of 4mm and a length of 2m;4.3.2.4 Chromatographic data processor: Shimadzu C-R6A or data processor with equivalent performance;4.3.2.5 Micro syringe: 10μL.
4.3.3 Preparation of chromatographic column
4.3.3.1 Filler
Carrier: 101 white carrier, particle size of 250~180μm Stationary liquid: succinic acid ethanol polyester (PEGS) Liquid phase loading: 3%.
4.3.3.2 Coating of fixative
Weigh 0.42g PEGS into a 250mL beaker, add chloroform solvent equivalent to the volume of 14g carrier, dissolve the fixative under an infrared lamp, then slowly pour 14g of the dried support into the beaker, place the beaker in a vacuum desiccator, keep it at a vacuum degree of about 80kPa for 5 to 10 minutes, take it out and place it in a fume hood, and allow the solvent to evaporate slowly under an infrared lamp until it is dry (tap the beaker frequently) to ensure uniform coating.
4.3.3.3 Filling method
Plug the copper mesh at one end of the chromatographic column connected to the detector, connect it to a vacuum pump, and connect a funnel to the other end. Slowly pour the stationary phase into the column under a vacuum of about 80kPa, and gently tap the chromatographic column until the stationary phase is no longer drawn into the column (the column is filled with about 12 people). Remove the chromatographic column, take out the copper mesh, add some stationary phase, plug the two ends of the chromatographic column with glass wool, and prepare for aging. 4.3.3.4 Chromatographic column aging
Put the filled chromatographic column in the column box of the chromatographic instrument, pass nitrogen (flow rate 5-20mL/min) and age it at 160℃ for 8h. 4.3.4 Chromatograph operating conditions
Select the optimal operating conditions according to different instruments and the requirements of this experiment. Taking Shimadzu GC-14A gas chromatograph and C-R6A data processor as an example, the operating conditions are as follows:
Column box temperature: 140℃;Www.bzxZ.net
Detector temperature: 220℃;
Vaporization chamber temperature: 280℃;
Carrier gas (nitrogen) flow rate: 50mL/min; Combustion gas (hydrogen) flow rate: 45mL/minAuxiliary gas (air) flow rate: 480mL/min2
W. paper speed: 2mm/min;
Injection volume: 0.6μL,
HG/T2669—95
Separation degree: R≥1.2 (m-aminoanisole and o-nitroanisole). 4.3.5 Preparation of calibration solution and determination of relative correction factor 4.3.5.1 Reagents
o-Anisidine: no impurities should be detected under the test conditions; p-Anisidine: content greater than 99%
m-Anisidine: content greater than 99%;
o-Nitroanisole: content greater than 99%;
o-Chloroaniline: content greater than 99%;
Chloroform (GB/T682).
4.3.5.2 Preparation of calibration solution
Solution A: weigh about 0.1g (accurate to 0.0002g) of o-chloroaniline in a 25mL volumetric flask, dilute to the mark with chloroform, mix well, and set aside.
Liquid B: Weigh about 0.1g (accurate to 0.0002g) of p-aminoanisole in a 25mL volumetric flask, dilute to the mark with chloroform, mix well, and set aside.
Liquid C: Weigh about 0.15g (accurate to 0.0002g) of m-aminoanisole in a 25mL volumetric flask, dilute to the mark with chloroform, mix well, and set aside.
Liquid D: Weigh about 0.15g (accurate to 0.0002g) of o-nitroanisole in a 25mL volumetric flask, dilute to the mark with chloroform, mix well, and set aside.
Liquid E: Weigh about 6g (accurate to 0.0002g) of o-aminoanisole in a 25mL volumetric flask, dilute to the mark with chloroform, mix well, and set aside.
Pipette the above solutions into 4 numbered 10mL volumetric flasks according to the provisions of Table 2, and mix them to obtain standard solutions No. 1, 2, 3, and 4.
Amount of solution added
Solution name
Volume after dilution with chloroform (mL)
Volume flask number
4.3.5.3 Determination of relative correction factor
After the operating conditions of the instrument are stable, use a micro-syringe to draw 0.6L of calibration solution and inject it into the vaporization chamber of the chromatograph. After the peaks are completely discharged, use the chromatographic data processor to automatically process and list the correction factors or accurately measure the peak area of each component (see the chromatogram). The relative correction factor f of each component is calculated according to formula (1): 3
W.bzsoso, cOmWhere: m——the mass of component i, mg; HG/T2669-95
mi·A.
m. ·A
A. Peak area of o-aminoanisole, mm2m. —Mass of o-aminoanisole, mg; A——Peak area of component i, mm2.
Note: The relative correction factor is recalibrated every week. 4.3.6 Determination steps
Pipette 0.55mL of sample into a 10mL volumetric flask, dilute to scale with chloroform, and mix well. Pipette 0.6μL of sample solution with a micro syringe and inject it into the vaporization chamber of the chromatograph. After the peak is completely discharged, use the chromatographic data processor to automatically process it, print out the analysis report or accurately measure the peak area of each component.
4.3.7 Calculation of analysis results
The mass percentage X of each component is calculated according to formula (2): X
Where: f——Relative correction factor of component i #Ar——Peak area of component i, mm2
——Water mass percentage.
4.3.8 Allowable difference
x(100—w)...
E（fi·A)
The difference between the results of two parallel determinations shall not exceed 0.2% for o-aminoanisole, and not exceed 0.2% for o-chloroaniline and p-aminoanisole.07%. Take the arithmetic mean as the analysis result.
① Low boiling point refers to all components eluting from the solvent peak to the main peak except o-chloroaniline, and its correction factor is calculated based on o-chloroaniline; ② High boiling point refers to all components eluting from the main peak except p-aminoanisole, and the correction factor of unknown components is calculated based on p-aminoanisole. 4.3.9 Chromatogram
See Figure 1 for the chromatogram.
Figure 1 Chromatogram of aminoanisole
1-Solvent: 2-o-aminoaniline, 3-o-hydroanisole 4-p-hydroanisole: 5-m-aminoanisole: 6-o-nitrobenzene 4.4 Determination of water content
Weigh 2-5g (accurate to 0.1g) of the sample, the solvent is a mixture of chloroform-methanol (3+1), and proceed according to the relevant provisions of GB/T13753.
W.bzsoso：com5 Inspection rules
HG/T2669—95
All items specified in Table 1 are factory inspection items. 5.1 Factory inspection
O-aminoanisole shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all o-aminoanisole shipped out of the factory meets the requirements of this standard. Each batch of o-aminoanisole shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 User acceptance
The user unit has the right to inspect the o-aminoanisole received in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.3 Sampling method
Randomly sample 10% of the barrels in each batch of products (with homogeneous products as one batch). Small batches of products shall not be less than 3 barrels. When sampling, use a glass tube with a diameter of 13mm and a length of 1m with a thinner end to probe from the barrel, including the upper, middle and lower parts of the sample. The sampling volume shall not be less than 500mL. Mix the sample carefully, divide it into two clean, dry, ground brown narrow-mouth bottles, and seal them with paraffin. Stick labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference. 5.4 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, re-sample from twice the amount of packaging for inspection. If the result of the re-inspection does not meet the requirements of this standard even if only one indicator does not meet the requirements of this standard, the entire batch of o-aminoanisole is unqualified. 5.5 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis should be conducted in accordance with the test methods specified in this standard.
6 Marking, packaging, transportation and storage
6.1 Marking
The packaging container of o-aminoanisole should be painted with firm and clear markings, including: manufacturer name, product name, registered trademark, specifications, standard number, production date, batch number, tare weight, net weight and toxicity mark. 6.2 Packaging
O-aminoanisole is packaged in 200L iron barrels, with a net weight of 200kg per barrel. 6.3 Transportation
Do not approach fire sources during transportation. Be careful when handling. O-aminoanisole is toxic and must not come into contact with skin or be inhaled into the body. Labor protection equipment must be worn during transportation, and strict safety precautions must be taken. 6.4 Storage
O-aminoanisole should be stored in a cool and dry warehouse, fireproof and sun-proof. Additional instructions:
This standard is proposed by the Technical Supervision 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 the Dye Factory of Jilin Chemical Industry Company. The main drafters of this standard are Xu Xiangyun and Fan Fang. From the date of implementation of this standard, the original national standard GB1065989 "O-aminoanisole" will be invalid. 5
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