CN111398488A - Content determination method of 2-ethoxyethylamine - Google Patents
Content determination method of 2-ethoxyethylamine Download PDFInfo
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- CN111398488A CN111398488A CN202010379027.1A CN202010379027A CN111398488A CN 111398488 A CN111398488 A CN 111398488A CN 202010379027 A CN202010379027 A CN 202010379027A CN 111398488 A CN111398488 A CN 111398488A
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- Prior art keywords
- temperature
- hydrogen
- chromatographic column
- ethoxyethylamine
- detection
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- BPGIOCZAQDIBPI-UHFFFAOYSA-N 2-ethoxyethanamine Chemical compound CCOCCN BPGIOCZAQDIBPI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012159 carrier gas Substances 0.000 claims abstract description 10
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000010453 quartz Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 abstract description 4
- 229940093475 2-ethoxyethanol Drugs 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000575 pesticide Substances 0.000 description 7
- 238000011161 development Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- SQDFHQJTAWCFIB-UHFFFAOYSA-N n-methylidenehydroxylamine Chemical compound ON=C SQDFHQJTAWCFIB-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000004009 herbicide Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- VOLGAXAGEUPBDM-UHFFFAOYSA-N $l^{1}-oxidanylethane Chemical compound CC[O] VOLGAXAGEUPBDM-UHFFFAOYSA-N 0.000 description 1
- 241000700159 Rattus Species 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a detection method, in particular to a content determination method of 2-ethoxy ethylamine, which adopts a thermal conductivity detector or a hydrogen flame ionization detector for detection, and the detection conditions are as follows: the thermal conductivity detector carrier gas is hydrogen, the hydrogen flame ionization detector carrier gas is nitrogen or hydrogen, and a certain chromatographic column DB-1701 is selected, the length is 60 meters, the diameter is 0.32mm, and the film thickness is 1.0 um. The flow rate of the column is 3ml/min, the sample injection temperature is 160-; the invention has the advantages of small dead volume of the capillary column, high detection sensitivity, good separation of 2-ethoxyethylamine, 2-ethoxyethanol and other organic impurities by selecting a specific chromatographic column, small tailing of chromatographic peak, good reproducibility of the method, and improved scientificity, advancement and applicability of the determination method.
Description
Technical Field
The invention relates to a content determination method of 2-ethoxyethylamine, in particular to a content determination method of 2-ethoxyethylamine.
Background
2-Ethoxyethylamine, 2-ethoxyyethyylamine, formula CH3CH2O(CH2)2NH2And the molecular weight is 89.14, and the water-soluble ammonia-free water-soluble organic solvent is a colorless transparent liquid, is miscible with water, is soluble in most organic solvents such as ethanol and has the odor of ammonia and is strong in alkalinity. Relative density (d20) of 0.85-0.86g/cm3The viscosity is low, the boiling point is 105 ℃, the freezing point is lower than-18 ℃, the refractive index (n20D) is 1.4080-1.4110, the flash point (closed cup) is 64 ℃, the pesticide is combustible, the toxicity is low, and half of death amount (rats) is L D50:1470mg/kg through mouth, L D50:2000mg/kg through skin, L C50:5.9753 mg/L is inhaled, the corrosive 2-ethoxyethylamine is an intermediate of pesticide herbicides and pharmaceutical chemicals, at present, green food and green life become pursuits of people, the use of high-efficiency, low-toxicity and low-residue pesticides becomes a development trend, the new generation oxime ether (ester) pesticides, bactericides and herbicides have similar characteristics, the oxime ether (ester) pesticides has wide development and application prospects as a novel pesticide, the application of the oxime ether (ester) pesticides is continuously expanded along with the development of society and science and technology, and the company is produced and sold at present in China.
At present, no literature exists on a method for measuring the content of 2-ethoxyethylamine.
Disclosure of Invention
The invention aims to solve the technical problem of providing a content determination method of 2-ethoxyethylamine.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a content determination method of 2-ethoxy ethylamine adopts a thermal conductivity detector or a hydrogen flame ionization detector for detection, and the detection conditions are as follows: the carrier gas of the thermal conductivity detector is hydrogen, the carrier gas of the hydrogen flame ionization detector is nitrogen or 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 sample injection temperature is 160-.
Preferably, in the method for measuring the content of 2-ethoxyethylamine, the chromatographic column is a DB-1701 quartz capillary chromatographic column, the length is 60 meters, the diameter is 0.32mm, and the film thickness is 1.0 um.
Preferably, in the method for measuring the content of 2-ethoxyethylamine, the sample injection temperature is 200 ℃, the initial column temperature is 60 ℃, the temperature is kept for 1 minute, the temperature is increased at the rate of 6 ℃/min by adopting a program, the final temperature is 200 ℃, the temperature is kept for 5 minutes, the detection temperature is 220 ℃, and the sample injection amount is 0.4 ul.
Has the advantages that: the invention has the advantages that:
the content determination method of the 2-ethoxyethylamine comprises the steps of groping specific determination conditions, repeatedly testing and screening, determining the main content of the 2-ethoxyethylamine by using a gas chromatography, adopting a capillary column with small dead volume and high detection sensitivity, selecting a specific chromatographic column to enable the 2-ethoxyethylamine, the 2-ethoxyethanol and other organic impurities to be better separated, having small tailing of chromatographic peaks and good reproducibility of the method, improving the scientificity, advancement and applicability of the determination method, particularly enabling the 2-ethoxyethylamine and the 2-ethoxyethanol to be separated under the condition of different contents, facilitating detection and analysis, being more accurate in precision, being directly used for guiding field production, and being capable of guiding the adjustment of field production process parameters more quickly to provide objective data information for production.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific examples.
Example 1
A content determination method of 2-ethoxy ethylamine adopts a thermal conductivity detector or a hydrogen flame ionization detector for detection, and the detection conditions are as follows: the thermal conductivity detector carrier gas is hydrogen, and the hydrogen flame ionization detector carrier gas is nitrogen or hydrogen. The chromatographic column adopts a quartz capillary tube as a material, and the flow rate of the chromatographic column is 3 ml/min. The sample introduction temperature is 200 ℃, the initial column temperature is 60 ℃, the temperature is kept for 1 minute, the temperature is raised at the speed of 6 ℃/min by adopting a program, the final temperature is 200 ℃, the temperature is kept for 5 minutes, the detection temperature is 220 ℃, and the sample introduction amount is 0.4 ul.
Determination of 2-The content of ethoxyethylamine was measured 10 times in parallel, and the result was found to be sample 1#X is 99.82% on average, relative standard deviation RSD is 0.02%, sample 2#The average of X is 99.62% and the relative standard deviation RSD is 0.04%, and the results of the two samples meet the requirements of the regulation. The method proves that the content of the 2-ethoxyethylamine is determined by adopting the gas chromatography, the 2-ethoxyethylamine, the 2-ethoxyethanol and other organic impurities can be better separated by selecting a specific method and a chromatographic column, the reproducibility of the method is good, and the measured content value of the 2-ethoxyethylamine is more accurate in precision.
Example 2
A content determination method of 2-ethoxy ethylamine comprises the following detection conditions: the sample introduction temperature is 160 ℃, the initial column temperature is 50 ℃, the temperature is kept for 1 minute, the temperature is raised by adopting a program at the speed of 6 ℃/min, the final temperature is 170 ℃, the temperature is kept for 5 minutes, the detection temperature is 180 ℃, and the sample introduction amount is 0.4 ul.
Example 3
A content determination method of 2-ethoxy ethylamine comprises the following detection conditions: the sample introduction temperature is 180 ℃, the initial column temperature is 70 ℃, the temperature is kept for 1 minute, the temperature is raised at the speed of 6 ℃/min by adopting a program, the final temperature is 190 ℃, the temperature is kept for 5 minutes, the temperature is detected to be 210 ℃, and the sample introduction amount is 0.4 ul.
Example 4
A content determination method of 2-ethoxy ethylamine comprises the following detection conditions: the sample introduction temperature is 190 ℃, the initial column temperature is 90 ℃, the temperature is kept for 1 minute, the temperature is raised by adopting a program at the speed of 6 ℃/min, the final temperature is 210 ℃, the temperature is kept for 5 minutes, the detection temperature is 220 ℃, and the sample introduction amount is 0.4 ul.
The chromatographic column used in the above examples 1-4 is a DB-1701 quartz capillary chromatographic column, the length is 60 meters, the diameter is 0.32mm, the film thickness is 1.0um, the chromatographic column using the quartz capillary as the material is also used in the examples 2-4, the column flow rate is 3ml/min, the detection is carried out by using a thermal conductivity detector or a hydrogen flame ionization detector, the carrier gas of the thermal conductivity detector is hydrogen, and the carrier gas of the hydrogen flame ionization detector is nitrogen or hydrogen.
The method for measuring the content of 2-ethoxyethylamine proposed in the patent of the invention is described in detail by referring to preferred examples, wherein the parts not described in detail are common knowledge of those skilled in the art. 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 content determination method of 2-ethoxy ethylamine is characterized in that: detecting by adopting a thermal conductivity detector or a hydrogen flame ionization detector under the following detection conditions:
the carrier gas of the thermal conductivity detector is hydrogen, the carrier gas of the hydrogen flame ionization detector is nitrogen or 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 sample injection temperature is 160-.
2. The method for measuring the content of 2-ethoxyethylamine according to claim 1, wherein: the chromatographic column is a DB-1701 quartz capillary chromatographic column, the length is 60 meters, the diameter is 0.32mm, and the film thickness is 1.0 um.
3. The method for measuring the content of 2-ethoxyethylamine according to claim 1, wherein: the sample introduction temperature is 200 ℃, the initial column temperature is 60 ℃, the temperature is kept for 2 minutes, the temperature is increased at the speed of 6 ℃/min, the final temperature is 200 ℃, the temperature is kept for 5 minutes, the detection temperature is 220 ℃, and the sample introduction amount is 0.4 ul.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010379027.1A CN111398488A (en) | 2020-05-07 | 2020-05-07 | Content determination method of 2-ethoxyethylamine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010379027.1A CN111398488A (en) | 2020-05-07 | 2020-05-07 | Content determination method of 2-ethoxyethylamine |
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| CN111398488A true CN111398488A (en) | 2020-07-10 |
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|---|---|---|---|
| CN202010379027.1A Pending CN111398488A (en) | 2020-05-07 | 2020-05-07 | Content determination method of 2-ethoxyethylamine |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328130A (en) * | 2008-07-24 | 2008-12-24 | 浙江新化化工股份有限公司 | Preparation of 2-ethoxy ethyl amine |
| US20130140449A1 (en) * | 2011-12-05 | 2013-06-06 | J. Fred Banks | Methods for detecting reverse triiodothyronine by mass spectrometry |
-
2020
- 2020-05-07 CN CN202010379027.1A patent/CN111398488A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328130A (en) * | 2008-07-24 | 2008-12-24 | 浙江新化化工股份有限公司 | Preparation of 2-ethoxy ethyl amine |
| US20130140449A1 (en) * | 2011-12-05 | 2013-06-06 | J. Fred Banks | Methods for detecting reverse triiodothyronine by mass spectrometry |
Non-Patent Citations (5)
| Title |
|---|
| CHAUDHARY, ADITYA等: "A GC-MS based metabolic profiling of probiotic lactic acid bacteria isolated from traditional food products", 《JOURNAL OF PURE AND APPLIED MICROBIOLOGY》 * |
| CHU JIN-FENG等: "Synthesis of Hydrochloride of Bis ( dimethoxypropylphosphinoethyl) -ethoxyethylamine", 《CHEMICAL JOURNAL OF CHINESE UNIVERSITIES-CHINESE》 * |
| 兰昭洪: "2-乙氧基乙醇氨化合成2-乙氧基乙胺工艺研究", 《精细化工中间体》 * |
| 粟学俐: "全二维气相色谱技术测定啤酒挥发组分", 《荆门职业技术学院学报》 * |
| 覃泰群等: "染料中间体γ-甲氧基丙胺的气相色谱分析", 《染料与染色》 * |
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Application publication date: 20200710 |