CN109725070B - Method for measuring content of N- (2-methoxycyclohexyl) -1,3-propane diamine - Google Patents
Method for measuring content of N- (2-methoxycyclohexyl) -1,3-propane diamine Download PDFInfo
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- CN109725070B CN109725070B CN201711053894.0A CN201711053894A CN109725070B CN 109725070 B CN109725070 B CN 109725070B CN 201711053894 A CN201711053894 A CN 201711053894A CN 109725070 B CN109725070 B CN 109725070B
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Abstract
The invention provides a method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine, which adopts a thermal conductivity detector to detect, wherein the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column DB-1301 made of quartz capillary, the length of the chromatographic column is 60 meters, the diameter of the chromatographic column is 0.32mm, and the film thickness of the chromatographic column is 1.05um. The flow rate of the column is 3ml/min, the initial column temperature is 60-80 ℃, the temperature is raised by adopting a program at the speed of 10 ℃/min, the final temperature is 250-. The method has the advantages that the specific determination conditions are searched, the gas chromatography is adopted to determine the content of the product, and the specific chromatographic column is selected to ensure that the N- (2-methoxycyclohexyl) -1,3-propane diamine, the solvent and other organic impurities can be better separated, the method has high accuracy and good reproducibility, so that the determination method has more scientificity, advancement, applicability and economy.
Description
Technical Field
The invention relates to a method for measuring the content of higher amine, in particular to a method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine.
Background
The propane diamine is N- (2-methoxycyclohexyl) -1,3-propane diamine, N- (2-methoxycyclohexyl) -1,3-propane diamine is N- (2-methoxycyclohexyl) -1,3-propane diamine, English name is N- (2-methoxycyclohexyl) -1,3-propane diamine, and molecular formula is C10H22N2O, molecular weight 186.29, is a colorless transparent liquid, miscible with water, and soluble in most organic solvents such as ethanol. Slightly ammoniacal smell. Is strongly alkaline. The relative density (d20) was 0.95. + -. 0.1. Low viscosity, boiling point 288.2 +/-30 deg.C. The freezing point is lower than-18 ℃. Refractive index (n20D) 1.478. No flash-off was observed at a flash point (closed cup) of 93 ℃. And is combustible. Low toxicity, half lethal dose (rats): the oral LD50 is 926mg/kg, the percutaneous LD50 is 1470mg/kg, and the inhaled LC50 is more than 5.1937 mg/L. It is corrosive.
At present, no literature exists for a method for measuring the content of N- (2-methoxycyclohexyl) -1, 3-propanediamine.
Disclosure of Invention
The invention provides the following technical scheme:
in order to solve the technical problems, the technical scheme of the invention is as follows:
a method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine is characterized in that: adopting a thermal conductivity detector for detection, wherein the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column taking a quartz capillary tube as a material, the flow rate of the chromatographic column is 3ml/min, the initial column temperature is 60-80 ℃, the temperature is raised at the speed of 10 ℃/min by adopting a program, the final temperature is 250-.
Preferably, in the content determination method of N- (2-methoxycyclohexyl) -1,3-propanediamine, the chromatographic column is a quartz capillary chromatographic column, the length is 60 meters, the diameter is 0.32mm, and the film thickness is 1.05um.
Preferably, in the content determination method of N- (2-methoxycyclohexyl) -1,3-propane diamine, the initial column temperature is 80 ℃, the initial column temperature is kept for 1 minute, the temperature is raised by adopting a program at a speed of 10 ℃/min, the final column temperature is 250 ℃, the final column temperature is kept for 18 minutes, the detection temperature is 280 ℃, the sample injection temperature is 280 ℃, and when a sample is tested, the anhydrous ethanol with the same volume and the sample are uniformly mixed, and the sample injection amount is 1 ul.
The invention has the advantages that:
the content determination method of the N- (2-methoxycyclohexyl) -1,3-propane diamine adopts the gas chromatography to determine the content of the N- (2-methoxycyclohexyl) -1,3-propane diamine, the inventor carries out extensive research experiments, repeatedly tests and screens by groping specific determination conditions, adopts a capillary column with small dead volume and high detection sensitivity, selects a specific chromatographic column to better separate the N- (2-methoxycyclohexyl) -1,3-propane diamine, solvent and other organic impurities, has good reproducibility of the method, ensures that the determination method has scientificity, advancement, applicability and economy, has more accurate determined content value precision of the 2-methoxycyclohexylamine, and can be directly used for guiding field production, the adjustment of the field production process parameters can be guided more quickly, and objective data information is prepared for production. The invention also prolongs the daily maintenance period of the instrument to a certain extent, reduces the maintenance cost of the instrument and improves the detection efficiency.
Detailed Description
The present invention will be described in further detail with reference to examples, which are illustrative of the present invention and are not to be construed as being limited thereto.
Example 1
A method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine adopts a thermal conductivity detector for detection, and the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column made of a quartz capillary tube, the flow rate of the chromatographic column is 3ml/min, the initial column temperature is 80 ℃, the temperature is kept for 1 minute, the temperature is raised at the speed of 10 ℃/min by adopting a program, the final temperature is 250 ℃, the temperature is kept for 18 minutes, the detection temperature is 280 ℃, the sample injection temperature is 280 ℃, and when a sample is tested, the anhydrous ethanol with the same volume and the sample are uniformly mixed, and the sample injection amount is 1 ul.
The content of N- (2-methoxycyclohexyl) -1,3-propanediamine is determined by gas chromatography, and the result is obtained after 10 times of parallel determination, namely a sample 1#X is 99.28% on average, relative standard deviation RSD is 0.04%, sample 2#The X average is 99.30% relative standard deviation RSD is 0.04% the results of the two samples meet the requirements. The method proves that the content of the N- (2-methoxycyclohexyl) -1,3-propanediamine is determined by adopting the gas chromatography, the N- (2-methoxycyclohexyl) -1,3-propanediamine, a solvent and other organic matter impurities, namely low-boiling-point substances and high-boiling-point substances can be better separated by selecting a specific chromatographic column, the reproducibility of the method is good, and the measured content value of the N- (2-methoxycyclohexyl) -1,3-propanediamine is more accurate in the aspect of precision.
Example 2
A method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine adopts a thermal conductivity detector for detection, and the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column made of a quartz capillary tube, the flow rate of the chromatographic column is 3ml/min, the initial column temperature is 60 ℃, the temperature is kept for 1 minute, the temperature is raised at the speed of 10 ℃/min by adopting a program, the final temperature is 255 ℃, the temperature is kept for 18 minutes, the detection temperature is 260 ℃, the sample injection temperature is 260 ℃, and when a sample is tested, the anhydrous ethanol with the same volume and the sample are uniformly mixed, and the sample injection amount is 1 ul.
Example 3
A method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine adopts a thermal conductivity detector for detection, and the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column made of a quartz capillary tube, the flow rate of the chromatographic column is 3ml/min, the initial column temperature is 60 ℃, the temperature is kept for 1 minute, the temperature is raised at the speed of 10 ℃/min by adopting a program, the final temperature is 260 ℃, the temperature is kept for 18 minutes, the detection temperature is 270 ℃, the sample injection temperature is 270 ℃, and when a sample is tested, the anhydrous ethanol with the same volume and the sample are uniformly mixed, and the sample injection amount is 1 ul.
Example 4
A method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine adopts a thermal conductivity detector for detection, and the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column made of a quartz capillary tube, the flow rate of the chromatographic column is 3ml/min, the initial column temperature is 65 ℃, the temperature is kept for 1 minute, the temperature is raised by adopting a program at the speed of 10 ℃/min, the final temperature is 265 ℃, the temperature is kept for 18 minutes, the detection temperature is 275 ℃, the sample injection temperature is 275 ℃, and when a sample is tested, the anhydrous ethanol with the same volume and the sample are uniformly mixed, and the sample injection amount is 1 ul.
The column used in examples 1 to 4 was a DB-1301 quartz capillary column, 60 m in length, 0.32mm in diameter, and 1.05um. in film thickness.
The method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine provided by the invention is described in detail by preferably referring to the implementation examples, wherein the parts which are not described in detail are the common knowledge of the technicians in the field. The scope of the present invention is defined by the appended claims, and all changes and modifications that come within the spirit of the invention or the meaning of the following claims are intended to be embraced therein.
Claims (3)
1. A method for measuring the content of N- (2-methoxycyclohexyl) -1,3-propane diamine is characterized in that: adopting a thermal conductivity detector for detection, wherein the detection conditions are as follows: the carrier gas is hydrogen, the chromatographic column adopts a chromatographic column taking DB-1301 quartz capillary as a material, the flow rate of the chromatographic column is 3ml/min, the initial column temperature is 60-80 ℃, the temperature is raised by adopting a program at the rate of 10 ℃/min, the final temperature is 250-.
2. The method for determining the content of N- (2-methoxycyclohexyl) -1,3-propanediamine according to claim 1, characterized in that: the length of chromatographic column is 60 meters, the diameter is 0.32mm, and the membrane thickness is 1.05um.
3. The method for determining the content of N- (2-methoxycyclohexyl) -1,3-propanediamine according to claim 1, characterized in that: the initial column temperature is 80 ℃, the initial column temperature is kept for 1 minute, the temperature is raised by adopting a program at the speed of 10 ℃/min, the final temperature is 250 ℃, the initial column temperature is kept for 18 minutes, the detection temperature is 280 ℃, the sample injection temperature is 280 ℃, and when a sample is tested, the equal volume of absolute ethyl alcohol and the sample are uniformly mixed, and the sample injection amount is 1 ul.
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Citations (3)
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| SU1608574A1 (en) * | 1989-01-03 | 1990-11-23 | Чебоксарское производственное объединение "Химпром" | Method of modifying hard carriers for gas chromatography |
| CN105486846A (en) * | 2015-12-24 | 2016-04-13 | 上海微谱化工技术服务有限公司 | Separating and detecting method for an amine antioxidant in butadiene styrene rubber |
| CN106866431A (en) * | 2017-02-22 | 2017-06-20 | 浙江新化化工股份有限公司 | A kind of production method of 1,3 propane diamine of N (2 methoxycyclohexyl) |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1608574A1 (en) * | 1989-01-03 | 1990-11-23 | Чебоксарское производственное объединение "Химпром" | Method of modifying hard carriers for gas chromatography |
| CN105486846A (en) * | 2015-12-24 | 2016-04-13 | 上海微谱化工技术服务有限公司 | Separating and detecting method for an amine antioxidant in butadiene styrene rubber |
| CN106866431A (en) * | 2017-02-22 | 2017-06-20 | 浙江新化化工股份有限公司 | A kind of production method of 1,3 propane diamine of N (2 methoxycyclohexyl) |
Non-Patent Citations (2)
| Title |
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| Quantitation method of N,N "-disalicylidene-1,2-propanediamine by comprehensive two-dimensional gas chromatography coupled to a nitrogen chemiluminescence detector;Lissitsyna, Kristina等;《JOURNAL OF SEPARATION SCIENCE》;20131231;第36卷(第11期);第1768-1773页 * |
| 气相色谱内标法测定1,3-丙二胺及其中间体的含量;杨俊峰等;《分析测试技术与仪器》;20081231(第03期);第176-178页 * |
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