CN109725070A - A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine - Google Patents
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine Download PDFInfo
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- CN109725070A CN109725070A CN201711053894.0A CN201711053894A CN109725070A CN 109725070 A CN109725070 A CN 109725070A CN 201711053894 A CN201711053894 A CN 201711053894A CN 109725070 A CN109725070 A CN 109725070A
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- propane diamine
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Abstract
The present invention provides a kind of N- (2- methoxycyclohexyl) -1, the content assaying method of 3- propane diamine, it is detected using thermal conductivity detector (TCD), testing conditions are as follows: carrier gas is hydrogen, chromatographic column uses quartz capillary for the chromatographic column DB-1301 of material, 60 meters of length, diameter 0.32mm, film thickness 1.05um.Column flow 3ml/min, 60-80 DEG C of initial column temperature, using temperature programming, heated up with the rate of 10 DEG C/min, 250-270 DEG C of final temperature, it is kept for 18 minutes, 260-280 DEG C of temperature of detection, 260-280 DEG C of injector temperature, when sample test, isometric dehydrated alcohol and sample are uniformly mixed, sample volume 1ul.It is an advantage of the invention that by groping particular assay condition, assay is carried out to product using gas chromatography, specific chromatographic column is selected to make N- (2- methoxycyclohexyl) -1,3- propane diamine and solvent and other organic impurities can be separated preferably, method accuracy height, favorable reproducibility, make measuring method with more science, advanced, applicability, economy.
Description
Technical field
The present invention relates to a kind of content assaying method of higher amines, especially a kind of N- (2- methoxycyclohexyl) -1,3-
The content assaying method of propane diamine.
Background technique
So-called propane diamine is a kind of N- (2- methoxycyclohexyl) -1,3- propane diamine, N- (2- methoxy basic ring in the present invention
Hexyl) -1,3- propane diamine property, N- (2- methoxycyclohexyl) -1,3- propane diamine, English name N- (2-
Methoxycyclohexl) -1,3-Propanediamine, molecular formula C10H22N2O, molecular weight 186.29 are a kind of colourless
Prescribed liquid, it is miscible with water, it is dissolved in most of organic solvents such as ethyl alcohol.Micro- smell for having ammonia.In strong basicity.Relative density (d20)
0.95±0.1.Viscosity is low, and 288.2 ± 30 DEG C of boiling point.Freezing point is lower than -18 DEG C.Index of refraction (n20D) 1.478.Flash-point (closed-cup)
93 DEG C do not find flash burn.It is flammable.Low toxicity, median lethal dose (rat): LD50 of passing through mouth: 926mg/kg, percutaneous LD50:1470mg/
Kg sucks LC50 > 5.1937mg/L.It is corrosive.
At this stage, N- (2- methoxycyclohexyl) -1,3- propane diamine current document of content assaying method is not yet.
Summary of the invention
The present invention provides the following technical solution:
In order to solve the above technical problems, the technical scheme is that
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine, it is characterised in that: examined using thermal conductivity
It surveys device to be detected, testing conditions are as follows: carrier gas is hydrogen, and chromatographic column uses quartz capillary for the chromatographic column of material, column flow
3ml/min, using temperature programming, is heated up with the rate of 10 DEG C/min by 60-80 DEG C of initial column temperature, and 250-270 DEG C of final temperature,
It is kept for 18 minutes, detects 260-280 DEG C of temperature, 260-280 DEG C of injector temperature, when sample test, by isometric dehydrated alcohol
It is uniformly mixed with sample, sample volume 1ul.
Preferably, the content of the content assaying method of above-mentioned a kind of N- (2- methoxycyclohexyl) -1,3- propane diamine
Chromatographic column described in measuring method be quartz capillary chromatographic column, 60 meters of length, diameter 0.32mm, film thickness 1.05um.
Preferably, the content of the content assaying method of above-mentioned a kind of N- (2- methoxycyclohexyl) -1,3- propane diamine
Initial column temperature 80 described in measuring method DEG C is kept for 1 minute, using temperature programming, is heated up with the rate of 10 DEG C/min, most final temperature
250 DEG C of degree is kept for 18 minutes, detects 280 DEG C of temperature, and 280 DEG C of injector temperature, when sample test, by isometric dehydrated alcohol
It is uniformly mixed with sample, sample volume 1ul.
Present invention has the advantage that
The content assaying method of above-mentioned N- (2- methoxycyclohexyl) -1,3- propane diamine, using gas chromatography to N- (2-
Methoxycyclohexyl) -1,3- propane diamine progress assay, inventor conducts extensive research test, by specific survey
Fixed condition is groped, and repetition test screening, small using capillary column dead volume, detection sensitivity is high, selects specific chromatographic column
It separate N- (2- methoxycyclohexyl) -1,3- propane diamine and solvent and other organic impurities can preferably, method reproducibility
It is good, make measuring method with more science, advanced, applicability, economy, the content value of measured 2- methoxycyclohexyl amine
Precision aspect is more accurate, is directly used in and instructs produced on-site, will instruct faster the adjustment of produced on-site technological parameter, makes a living
It produces to provide and prepares objective data information.The present invention extends the instrument daily maintenance period to a certain extent simultaneously, reduces instrument
Device maintenance cost, improves detection efficiency.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, following embodiment be explanation of the invention and
The invention is not limited to following embodiments.
Embodiment 1
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine, is examined using thermal conductivity detector (TCD)
It surveys, testing conditions are as follows: carrier gas is hydrogen, and chromatographic column uses quartz capillary for the chromatographic column of material, column flow 3ml/min, just
It 80 DEG C of beginning column temperature, is kept for 1 minute, using temperature programming, is heated up with the rate of 10 DEG C/min, 250 DEG C of final temperature, kept for 18 points
Clock detects 280 DEG C of temperature, 280 DEG C of injector temperature, when sample test, isometric dehydrated alcohol and sample is uniformly mixed, into
Sample amount 1ul.
Using the content of gas chromatography measurement N- (2- methoxycyclohexyl) -1,3- propane diamine, by 10 parallel surveys
Determine as a result, sample 1#X average=99.28%, relative standard deviation RSD=0.04%, sample 2#The opposite mark of X average=99.30%
Two sample measurement results of quasi- deviation RSD=0.04% meet prescribed requirement.Prove the measuring method " using gas chromatography pair
N- (2- methoxycyclohexyl) -1,3- propane diamine carries out assay, and specific chromatographic column is selected to make N- (2- methoxycyclohexyl
Base) -1,3- propane diamine and solvent and other organic impurities low-boiling-point substances and high-boiling components can separate preferably, method favorable reproducibility,
Measured N- (2- methoxycyclohexyl) -1,3- propane diamine content value precision aspect is more accurate ".
Embodiment 2
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine, is examined using thermal conductivity detector (TCD)
It surveys, testing conditions are as follows: carrier gas is hydrogen, and chromatographic column uses quartz capillary for the chromatographic column of material, column flow 3ml/min, just
It 60 DEG C of beginning column temperature, is kept for 1 minute, using temperature programming, is heated up with the rate of 10 DEG C/min, 255 DEG C of final temperature, kept for 18 points
Clock detects 260 DEG C of temperature, 260 DEG C of injector temperature, when sample test, isometric dehydrated alcohol and sample is uniformly mixed, into
Sample amount 1ul.
Embodiment 3
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine, is examined using thermal conductivity detector (TCD)
It surveys, testing conditions are as follows: carrier gas is hydrogen, and chromatographic column uses quartz capillary for the chromatographic column of material, column flow 3ml/min, just
It 60 DEG C of beginning column temperature, is kept for 1 minute, using temperature programming, is heated up with the rate of 10 DEG C/min, 260 DEG C of final temperature, kept for 18 points
Clock detects 270 DEG C of temperature, 270 DEG C of injector temperature, when sample test, isometric dehydrated alcohol and sample is uniformly mixed, into
Sample amount 1ul.
Embodiment 4
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine, is examined using thermal conductivity detector (TCD)
It surveys, testing conditions are as follows: carrier gas is hydrogen, and chromatographic column uses quartz capillary for the chromatographic column of material, column flow 3ml/min, just
It 65 DEG C of beginning column temperature, is kept for 1 minute, using temperature programming, is heated up with the rate of 10 DEG C/min, 265 DEG C of final temperature, kept for 18 points
Clock detects 275 DEG C of temperature, 275 DEG C of injector temperature, when sample test, isometric dehydrated alcohol and sample is uniformly mixed, into
Sample amount 1ul.
Chromatographic column used in above-described embodiment 1-4 be DB-1301 quartz capillary chromatographic column, 60 meters of length, diameter 0.32mm,
Film thickness 1.05um..
A kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine proposed by the present invention, by compared with
Good is described in detail referring to examples of implementation, wherein the part that do not address in detail is the known normal of those skilled in the art
Know.Protection scope of the present invention is based on the contents of the claims, all based on technical inspiration of the invention or similar replacement
And change, the change and modification in the case where not departing from present general inventive concept should belong within protection scope of the present invention.
Claims (3)
1. a kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine, it is characterised in that: use Thermal Conductivity
Device is detected, testing conditions are as follows: carrier gas is hydrogen, and chromatographic column uses quartz capillary for the chromatographic column of material, column flow
3ml/min, using temperature programming, is heated up with the rate of 10 DEG C/min by 60-80 DEG C of initial column temperature, and 250-270 DEG C of final temperature,
It is kept for 18 minutes, detects 260-280 DEG C of temperature, 260-280 DEG C of injector temperature, when sample test, by isometric dehydrated alcohol
It is uniformly mixed with sample, sample volume 1ul.
2. a kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine according to claim 1, special
Sign is: the chromatographic column be quartz capillary chromatographic column, 60 meters of length, diameter 0.32mm, film thickness 1.05um.
3. a kind of content assaying method of N- (2- methoxycyclohexyl) -1,3- propane diamine according to claim 1, special
Sign is: 80 DEG C of the initial column temperature, is kept for 1 minute, using temperature programming, is heated up with the rate of 10 DEG C/min, final temperature
250 DEG C, kept for 18 minutes, detect 280 DEG C of temperature, 280 DEG C of injector temperature, when sample test, by isometric dehydrated alcohol and
Sample is uniformly mixed, sample volume 1ul.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114965778A (en) * | 2022-05-30 | 2022-08-30 | 江西威科油脂化学有限公司 | Method for determining palmitamide and stearamide in stearamide product |
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| 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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2017
- 2017-10-31 CN CN201711053894.0A patent/CN109725070B/en active Active
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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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| LISSITSYNA, KRISTINA等: "Quantitation method of N,N "-disalicylidene-1,2-propanediamine by comprehensive two-dimensional gas chromatography coupled to a nitrogen chemiluminescence detector", 《JOURNAL OF SEPARATION SCIENCE》 * |
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Cited By (2)
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| CN114965778A (en) * | 2022-05-30 | 2022-08-30 | 江西威科油脂化学有限公司 | Method for determining palmitamide and stearamide in stearamide product |
| CN114965778B (en) * | 2022-05-30 | 2023-11-17 | 江西威科油脂化学有限公司 | Determination method of palmitoyl acid amide and stearic acid amide in stearic acid amide product |
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