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Chemical Industry Standard of the People's Republic of China
HG/T2720-95
Published on June 30, 1995
Ministry of Chemical Industry of the People's Republic of China
Implemented on June 1, 1996
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2720-95
This standard specifies the technical requirements, test methods, inspection rules, and requirements for marking, packaging, transportation and storage of diethylamine. This standard applies to diethylamine 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: CHnN
Structural formula: CHs-CH2-NH-CH2-CHs
Relative molecular mass: 73.14 (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 diethylamine should meet the requirements of Table 1.
Diethylamine content, %
Ethylamine content, %
Triethylamine content, %
Ethanol content, %
Acetonitrile content, %
Water content, %
4 Test methods
4.1 Determination of appearance
1995-06-30 Approved by the Ministry of Chemical Industry of the People's Republic of China Superior products
First-class products
Qualified products
1996-06-01 Implementation
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4.2 Determination of diethylamine content and impurity content 4.2.1 Summary of the method
HG/T2720-95
Gas chromatography is used, and the area normalization method is used for quantitative determination to obtain the content of diethylamine and organic impurities. 4.2.2 Instruments
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;
Di-o-phthalate;
Solvent: Acetone (GB/T686).
4.2.3.2 The amount of the fixing solution applied: (56.75% polyethylene glycol 2000 + 40% diisocyanate + 3.25% triethanolamine) + 101 white support = 20 + 100.
4.2.3.3 Application of the fixing solution
Weigh 1.8g polyethylene glycol 2000, 1.28g diisocyanate, and 0.12g triethanolamine, put them in a 250mL beaker, add 35mL acetone to dissolve, pour 16g 101 white support into it to completely soak it, stir it gently, and slowly evaporate the solvent to dryness in a 50℃ water bath.
4.2.3.4 Filling method
Plug the detector end of the chromatographic column with a copper mesh, connect it to a vacuum pump, connect the other end to a funnel, 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
Put the filled chromatographic column in the column box of the chromatographic instrument, test for leaks, pass nitrogen (maintain a flow rate of 10mL/min), and age at 80℃ for 12h. During aging, the column should be disconnected from the detector. 4.2.4 Chromatograph operating conditionsbzxZ.net
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); Quantitative method: corrected area normalization method. 4.2.5 Preparation of standard solution
4.2.5.1 Reagents
HG/T2720—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;
acetonitrile: analytical grade.
4.2.5.2 Preparation of standard solution
The preparation method of standard solution is shown in Table 2.
Triethylamine
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 3μL of standard solutions 1 to 4 respectively 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 f of each component is calculated according to formula (1): fr
-relative correction factor of component i;
mass of component i, g;
mass of diethylamine, g;
Ai component peak area, mm;
peak area of diethylamine, mm.
Note: the relative correction factor of each component should be reviewed once a month. 4.2.7 Determination of sample
mXA.
Pipette 3μL of diethylamine 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 (chromatographic separation diagram 3
W.HG/T2720-95
see Figure 1), accurately measure the peak area of each component or calculate it automatically using the chromatographic processor. 4.2.8 Calculation of results
The content of each component is calculated according to formula (2):
X=fIXA)
Wherein, X, mass percentage of component i, %, fi——correction factor of component i;
A,—peak area of component i, mm.
4.2.9 Allowable difference
(2)
The difference between the two parallel determination results of diethylamine 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%. The arithmetic mean shall be taken as the analysis result. 4.2.10 Chromatogram
The chromatogram is shown in Figure 1.
Figure 1 Gas chromatogram of diethylamine
1——Ethylamine; 2—Diethylamine; 3—Triethylamine; 4—Ethanol, 5—Ethylamine; 6—Water 5 Inspection rules
All items specified in Table 1 are factory inspection items. 5.1 Factory inspection
Diethylamine shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all diethylamine shipped out of the factory meets the requirements of this standard. Each batch of diethylamine 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 inspect and accept the diethylamine received in accordance with the provisions of this standard to inspect 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 carried out 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, re-sampling shall be carried out from twice the amount of packaging. If the re-test results show that even if only one indicator does not meet the requirements of this standard, the entire batch of diethylamine shall be 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
Diethylamine packaging containers 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 in accordance with the provisions of GB190, "flammable" and "toxic" signs should be marked. 6.2 Packaging
Ethylamine is packaged in 200L closed steel drums or hard plastic drums, with a net weight of 140kg per barrel. 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
Diethylamine 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 was 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 were Wang Pinjiang, Gao Zhongmin, Zhou Shuqin, and Chen Yaqing. 5
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