Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2719-95
Published on 1995-06-30
Ministry of Chemical Industry of the People's Republic of China
Implemented on 1996-06-01
WChemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2719-95
This standard specifies the technical requirements, test methods, inspection rules, and requirements for marking, packaging, transportation and storage of monoethylamine. This standard applies to monoethylamine obtained by converting raw materials with high nickel catalyst and ethanol amination in the presence of hydrogen. This product is mainly used in pesticides, medicines, dyes and rubber processing. Molecular formula: CHN
Structural formula: CHs-CH2-NH2
Relative molecular weight: 45.08 (according to the international relative atomic mass in 1991) Reference standards
GB190 Dangerous goods packaging mark
GB/T6678 General rules for sampling of chemical products
GB/T6680 General rules for sampling of liquid chemical products GB/T9722
2 General rules for gas chromatography of chemical reagents
3 Technical requirements
3.1 Appearance: Colorless and transparent liquid, free of mechanical impurities. The quality of monoethylamine should meet the requirements of Table 1.
Monoethylamine content, %
Inorganic ammonia content, %
Triethylamine content, %
Triethylamine content, %
Ethanol content, %
Ethyl content, %
Moisture content, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on June 30, 1995Superior product
49.5~51.0
First-class product
49.5~51.0
Qualified product
49.5~51.0
Implemented on June 1, 1996
W.4 Test method
4.1 Determination of appearance
Visual determination is adopted.
4.2 Determination of monoethylamine content and impurity content 4.2.1 Method summary
HG/T271995
Gas chromatography is used to quantify the content of monoethylamine and organic impurities by area normalization method. 4.2.2 Instruments bZxz.net
Gas chromatograph: should meet the requirements of GB/T9722; Chromatographic column: 4000mm×3.5mm stainless steel column or glass column; Detector: Thermal conductivity detector (TCD);
Microprocessor or plotter: response time 1s; Micro syringe: 10μL.
4.2.3 Preparation of chromatographic column
4.2.3.1 Filler and reagents
Carrier: 101 white carrier, particle size 250~177μm (60~80 mesh); stationary liquid: polyethylene glycol 2000;
triethanolamine;
dichlorophthalate;
solvent: acetone (GB/T686).
4.2.3.2 The coating amount of stationary liquid: (56.75% polyethylene glycol 2000 + 40% dichlorophthalate + 3.25% triethanolamine) + 101 white carrier = 20 + 100.
4.2.3.3 Coating of stationary phase
Weigh 1.80g polyethylene glycol 2000, 1.28g di-orthophthalate, 0.12g triethanolamine, put them in a 250mL beaker, add 35mL acetone to dissolve, pour 16g 101 white support into it, make it completely soaked, stir gently, and slowly evaporate the solvent to dryness in a 50℃ water bath.
4.2.3.4 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 at the other end, slowly pour in the stationary phase, and gently tap the chromatographic column until the stationary phase is no longer drawn into the column (the column loading volume is about 17g), remove the chromatographic column, remove the copper mesh, add some stationary phase, plug the two ends of the chromatographic column with glass wool, and prepare for aging. 4.2.3.5 Aging of Chromatographic Column
Place the filled chromatographic column in the column box of the chromatograph, test for leaks, and age it at 80°C for 12 hours with nitrogen (maintaining a flow rate of 10 mL/min). During aging, the column should be disconnected from the detector. 4.2.4 Chromatograph operating conditions
Select the optimal operating conditions according to different instruments and the requirements of this experiment. Taking SP501N gas chromatograph as an example, the operating conditions are as follows: Column box temperature: 68±0.5℃;
Detector temperature: 110℃;
Vaporization chamber temperature: 130℃;
Carrier gas (hydrogen) flow rate: 55mL/min; Bridge flow: 200mA;
Paper speed: 300mm/h;
Injection volume: 3μL;
Amplifier attenuation: the main peak is attenuated by 1/64, and the other component peaks are attenuated by 1/4 (attenuated by 1/4 when using an integrator); 2
Quantitative method: corrected area normalization method. 4.2.5 Preparation of standard solution
4.2.5.1 Reagents
HG/T2719—95
Ethylamine: no impurities should be detected under the test conditions; Diethylamine: no impurities should be detected under the test conditions; Triethylamine: no impurities should be detected under the test conditions; Anhydrous ethanol: high-grade pure;
Ammonia water (25.3%): analytical grade (measure the exact content when using); Acetonitrile: analytical grade.
4.2.5.2 Preparation of standard solution
The preparation method of standard solution is shown in Table 2.
Monoethylamine
Diethylamine
Triethylamine
Anhydrous ethanol
Note: After the standard solution is prepared, it should be stored in the refrigerator for future use. 4.2.6 Determination of correction factor
After the instrument's operating conditions are stable, take 3uL of standard solutions No. 1 to No. 4 and inject them into the vaporization chamber of the chromatograph. At the same time, start the chromatographic data processor. After the peaks are completely discharged, accurately measure the peak area of each component or let the chromatographic processor automatically calculate the result. The relative correction factor of each component is calculated according to formula (1): fh
Wherein: f——relative correction factor of component i; mi
mass of component i, g;
mass of ethylamine, g;
WA—peak area of component i, mm;
A——peak area of monoethylamine, mm2.
Note: The relative correction factor of each component is reviewed once a month. 4.2.7 Determination of sample
HG/T271995
Take 3μL of monoethylamine sample and inject it into the vaporization chamber of the chromatograph. At the same time, start the chromatographic processor. After the peaks are completely discharged (see Figure 1 for the chromatographic separation diagram), accurately measure the peak area of each component or use the chromatographic processor to automatically calculate. 4.2.8 Calculation of results
The content of each component is calculated according to formula (2):
Xi=IXA)
Where: x——mass percentage of component i, %, f——correction factor of component i;
Ai component peak area, mm.
4.2.9 Allowable difference
(2)
The difference between the two parallel determination results of ethylamine content shall not exceed 0.2%, the difference between the other organic impurity components shall not exceed 0.02%, and the difference between the two determination results of water content shall not exceed 0.02%. Take their arithmetic mean as the analysis result. 4.2.10 Chromatogram
See Figure 1 for the chromatogram.
1—Inorganic ammonia; 2—
5 Inspection rules
Gas chromatogram of monoethylamine
Ethylamine; 3—
Diethylamine; 4—
Triethylamine; 5—Ethanol: 6—Acetonitrile: 7—Water All items specified in Table 1 are factory inspection items. 5.1 Factory inspection
Monoethylamine shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all monoethylamine shipped out of the factory meets the requirements of this standard. Each batch of monoethylamine shipped out of the factory shall be accompanied by a quality certificate in a certain format. Its contents include: manufacturer name, product name, grade, batch number, net weight, production date, product quality and standard number. 5.2 User Acceptance
The user unit has the right to accept the received monoethylamine in accordance with the provisions of this standard and check whether it meets the requirements of this standard. 5.3 Sampling method
Sampling shall be carried out in accordance with the provisions of GB/T6678 and GB/T6680. Sampling shall be taken from the top, middle and bottom with a sampling tube. The total sampling volume shall not be less than 500mL. The samples shall be divided into two clean and dry ground-mouth bottles and sealed with paraffin. Labels shall be affixed to the bottles, indicating: product name, batch, sampling date, name of the sampler. One bottle shall be inspected by the laboratory and the other bottle shall be sealed and stored for three months. 5.4 Re-test
If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. If only one indicator does not meet the requirements of this standard, the whole batch of monoethylamine 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, purchase and storage
6.1 Marking
The packaging container of monoethylamine should be painted with firm and clear markings, including: manufacturer name, product name, registered trademark, product grade, standard number, production date, batch number, tare weight, net weight. And according to the provisions of GB190, the "flammable" and "toxic" signs should be marked. 6.2 Packaging
Monoethylamine is packaged in 200L closed steel drums or hard plastic drums, with a net weight of 140kg per drum. 6.3 Transportation
The generation of static sparks should be reduced during transportation, and it is not allowed to come into contact with the skin during handling. 6.4 Storage
Monoethylamine should be stored in a clean, cool, dry warehouse away from fire sources, and protected from sunlight and rain. Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is jointly managed by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and the Beijing Chemical Research Institute. This standard was drafted by the Shenyang Chemical Research Institute and the Jiangcheng Dye Factory of Jilin Chemical Industry Corporation. The main drafters of this standard are Wang Pinjiang, Gao Zhongmin, Zhou Shuqin, and Chen Yaqing. 5
W.bzsoso.coI
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.