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Chemical Industry Standard of the People's Republic of ChinaWww.bzxZ.net
HG/T2816—1996
Industrial Cyclohexylamine
Published on June 28, 1996
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1997
WHG/T2816—1996
This standard's superior and first-class products are equivalent to the US military standard 0C-940B1975 "Cyclohexylamine", and three control indicators of aniline, dicyclohexylamine and moisture are added.
This standard uses gas chromatography instead of chemical method to determine the purity of cyclohexylamine, and can simultaneously determine the content of the main organic impurities of cyclohexylamine. This standard uses the Karl Fischer method specified in ISO760:1976 to determine the moisture content of cyclohexylamine. The superior products of this standard reach the technical level of foreign advanced standards, and the first-class products reach the general international level. This standard is the first industry standard formulated. Appendix A of this standard is the standard appendix.
Appendix B and Appendix C of this standard are indicative appendices. 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 jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Liang Zhishun.
W.bzsosO.cO1Scope
Chemical Industry Standard of the People's Republic of China
HG/T2816—1996
This standard specifies the requirements, sampling methods, test methods, marking, packaging, transportation and storage of industrial cyclohexylamine. This standard applies to cyclohexylamine prepared by catalytic hydrogenation of aniline at normal pressure. Molecular formula: CHiaN
Structural formula:
Relative molecular mass: 99.17 (according to the 1993 international relative atomic mass) 2Referenced 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 parties using this standard should explore the possibility of using the latest versions of the following standards. GB190-90 Dangerous Goods Packaging Marking
GB/T1250-89 Methods for expressing and determining limit values GB/T2366-86 Determination of moisture content in chemical products Gas chromatography GB/T6283-86 Determination of moisture content in chemical products Karl Fischer method (general method) (eqVISO760:1978)
GB/T6680-86 General rules for sampling of liquid chemical products 3 General rules for gas chromatography of chemical reagents
GB9722-88
3 Requirements
3.1 Appearance: Colorless or light yellow transparent liquid, without visible impurities. 3.2 Industrial cyclohexylamine shall meet the requirements of Table 1: Table 1
Cyclohexylamine
Dicyclohexylamine
Superior product
Ministry of Chemical Industry of the People's Republic of China Approved on 1996-06-28
First-class product
Qualified product
Implemented on 1997-01-01
W.bzsoso:com4 Sampling
4.1 Products with uniform quality are considered as one batch.
HG/T2816—1996
4.2 According to the provisions of Article 1.4 of GB/T6680, samples shall be collected from the packaging barrels of each batch of products. When sampling, use a glass tube with a diameter of about 10mm and a length of about 1m to take out samples from the upper, middle and lower parts of the packaging barrel. The total amount of samples shall not be less than 500mL. 4.3 After the samples are mixed evenly, they are placed in two clean and dry ground-mouth bottles. Labels are attached to the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is inspected by the inspection department, and the other bottle is sealed and kept for three months for future reference. 4.4 If one of the indicators does not meet the requirements of this standard in the inspection results, samples should be taken from the packaging barrels with twice the amount for re-inspection. Even if only one indicator does not meet the requirements of this standard in the re-inspection results, the entire batch of products is unqualified. 5 Test methods
5.1 Common matters
5.1.1 The reagents used in this standard are analytically pure reagents unless other requirements are specified. 5.1.2 The determination of the test results shall be based on the rounded value comparison method specified in GB/T1250. The final expression of the results shall be consistent with the required indicator value digits.
5.2 Appearance
Observe visually.
5.3 Determination of cyclohexylamine, aniline and dicyclohexylamine content 5.3.1 Method summary
The cyclohexylamine sample is separated from the impurities by passing through the chromatographic column, and then detected by the flame ionization detector and quantified by the normalization method. 5.3.2 Instruments
Gas chromatograph: sensitivity and stability meet the requirements of GB9722; chromatographic column: stainless steel column with an inner diameter of 3mm and a length of 2m; detector: flame ionization detector;
Recorder: chromatography data processor;
Injector: 1μL micro-syringe.
5.3.3 Filler
Fixed liquid: sodium dodecylbenzene sulfonate;
Carrier: white 101 silanized carrier, particle size 149～177μm (100～80 mesh), pretreated with 1% potassium hydroxide. Coating degree: fixed liquid/carrier = 5/100.
Coating of the fixing solution
Weigh 0.08g of potassium hydroxide in a 250mL beaker, add 25mL of methanol to dissolve it, slowly pour 8.0g of the dried carrier into the beaker to completely soak the carrier, soak it for 15min, heat it under an infrared lamp, gently tap and rotate the beaker to make the coating uniform, after the solvent evaporates, dry it in a 100℃ oven for about 30min. Weigh 0.40g of sodium dodecylbenzene sulfonate in a 250mL beaker, add 25mL of chloroform to dissolve it, slowly pour the treated carrier into the beaker to completely soak it, soak it for 30min, heat it under an infrared lamp, gently tap and rotate the beaker to make the coating uniform, after the solvent evaporates, dry it in a 100℃ oven for 30min. e) Filling method
Wrap the end of the chromatographic column connected to the detector with gauze, connect it to a vacuum pump, and connect the other end to a funnel. Slowly pour the freshly dried stationary phase into the column under vacuum to fill the column evenly and tightly (the column volume is about 6g). Plug the two ends of the filled column with glass wool and prepare for aging. f
Aging of chromatographic column
Put the filled chromatographic column into the column box of the chromatographic instrument, age it for 8 hours at a nitrogen flow rate of about 10mL/min and a column box temperature of 160℃. During aging, the chromatographic column should be disconnected from the detector. 5.3.4 Determination of correction factor
See Appendix A (Standard Appendix).
5.3.5 Chromatographic operating conditions
See Appendix B (Suggestive Appendix).
5.3.6 Analysis steps
HG/T2816—1996
Start the instrument, wait for all operating conditions to stabilize, draw 0.4uL of sample for injection, after the peak is eluted, the mass percentage of component i is calculated as follows.
Wherein, X——component i content, %;
X,=-ft:A×(100-w)
z·f·A)
\——component i peak area attenuation multiple; fi component i correction factor, mg/mm;
Ar——component i peak area, mm;
w—the percentage of moisture content measured according to 5.4. Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results of cyclohexylamine shall not exceed 0.2%. 5.4 Determination of moisture
5.4.1 Karl Fischer method (arbitration method) Determination of moisture shall be carried out in accordance with the method of GB/T6283. The arithmetic mean of the results of two parallel determinations shall be taken as the determination result, and the difference between the results of two parallel determinations shall not exceed 0.05%. 5.4.2 Chromatographic method
See Appendix C (suggestive appendix).
6 Marking, packaging, transportation and storage
6.1 The packaging container of cyclohexylamine shall be clearly marked with: manufacturer name, factory address, product name, trademark, net weight, production date, batch number, grade and this standard number, and in accordance with the provisions of GB190, the "flammable and corrosive product" mark shall be marked. 6.2 Cyclohexylamine shall be packaged in clean, dry and firm 200L steel drums, with a net weight of 170kg per drum. 6.3 During transportation and storage, it shall not be close to fire sources, and shall be protected from sun and rain. It shall be handled with care. 6.4 When operating, protective equipment must be used to avoid direct contact with the skin or inhalation. 3
W.bzsoso.Appendix A (Standard Appendix)
A1 Preparation of calibration mixed solution
a) Reagents
Cyclohexane;
Determination of correction factor
Cyclohexylamine: No impurities were detected under the test conditions of this standard; Aniline;
Dicyclohexylamine.
Preparation of single calibration solution
Weigh various reagents (accurate to 0.0002g) in a clean and dry 25mL volumetric flask according to Table A1, and dilute to the mark with cyclohexylamine. The shelf life of the single calibration solution is two months. Preparation of single calibration solution
Single calibration solution
Amount, g
Preparation of calibration mixed solution
Cyclohexane
Dicyclohexylamine
According to the requirements of Table A2, use a pipette to pipette the above single calibration solutions into a clean and dry 10mL volumetric flask of known mass, dilute to the scale with cyclohexylamine, mix well, and weigh the mass of the solution (accurate to 0.001g). The use period of the calibration mixed solution is one month. Table A2 Preparation of calibration mixed solution
Single calibration
Amount of solution added
Name of calibration solution
Determination and calculation of correction factor
Calibration mixed
Solution number
Start the chromatograph. After the operating conditions are stable, take 0.4uL of calibration mixed solution for injection. After the peak is eluted, calculate the correction factor of each component according to the following formula:
Wherein: f--correction factor of component i, mg/mmm
-mass of component i, mg;
A--peak area of component i, mm.
W.bzsoso.coIAppendix B (suggestive appendix)
Chromatographic operating conditions and spectra of cyclohexylamine, aniline and dicyclohexylamineB1Select appropriate chromatographic operating conditions according to the requirements of this standard. Taking HP5890 chromatograph as an example, the operating conditions are as follows: column box temperature: 125℃;
detection temperature: 250℃;
vaporization temperature: 250℃;
carrier gas (nitrogen) flow rate: 25mL/min; combustion gas (hydrogen) flow rate: 30mL/min; auxiliary gas (air) flow rate: 400mL/min; injection volume: 0.4μL;
paper speed: 300mm/h;
quantitative method: area normalization method;
resolution: above 1.0 (based on cyclohexylamine and aniline). B2 Standard sample chromatogram
Figure B1 Cyclohexylamine chromatogram
The components and relative retention times of each peak in Figure B1 are shown in Table B1. Table B1
Relative retention time
Cyclohexane
Cyclohexylamine
Dicyclohexylamine
W. Appendix C (Suggested Appendix)
Gas chromatography determination of water content in cyclohexylamine C1 The determination was carried out in accordance with the method of GB/T2366. The chromatographic conditions are as follows:
Chromatographic column: stainless steel column with an inner diameter of 3mm and a column length of 1m; Filling material: GDX-403 carrier, particle size 149~177μm (100~80 mesh); Column box temperature: 105℃;
Vaporization temperature: 250℃;
Bridge current: 160mA;
Carrier gas (hydrogen) flow rate: 35mL/min; Injection volume: 5μL.
The water chromatogram of cyclohexylamine is as follows:
1—water; 2—cyclohexylamine
Figure C1 Water chromatogram of cyclohexylamine
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