CN102553468A - Preparation method for ethyl nitrite standard air - Google Patents
Preparation method for ethyl nitrite standard air Download PDFInfo
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- CN102553468A CN102553468A CN2010106163926A CN201010616392A CN102553468A CN 102553468 A CN102553468 A CN 102553468A CN 2010106163926 A CN2010106163926 A CN 2010106163926A CN 201010616392 A CN201010616392 A CN 201010616392A CN 102553468 A CN102553468 A CN 102553468A
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Abstract
The invention provides a preparation method for ethyl nitrite standard air. The method comprises the following steps of: a 1, inducing inert gas into a clean sealed flexible container; a 2, injecting ethyl nitrite standard liquid into a clean sealed ampoule bottle through a micro-chromatograph sample-injecting needle; a 3, placing the ampoule bottle in a sealed container 2, and slowly flushing the container 2 by using the inert gas in the flexible container so as to exhaust the air in the container 2; a 4, pumping the container 2 until the pressure in the container 2 is negative, and sealing the container 2; a 5, shaking the container 2 forcefully to smash the ampoule bottle, after the ethyl nitrite is completely volatilized, continuously supplementing the inert gas into the container 2, and after the air pressure in the container 2 is in balance with the external atmosphere pressure, sealing the container 2 again; and a 6, shaking the container 2 slightly to fully mix air so as to prepare the ethyl nitrite standard air. The standard air prepared by the method is purer and more accurate and is more quickly prepared. The method is usually applied to fields, such as environment and medicine.
Description
[technical field]
The present invention relates to the field of prepared in laboratory calibrating gas, particularly a kind of preparation method of a small amount of nitrous ether (ethyl nitrite) calibrating gas.
[background technology]
Nitrous ether (ethyl nitrite) is colourless extremely faint yellow supernatant liquid, and special odor is arranged, and it is sweet to distinguish the flavor of, 17.2 ℃ of boiling points, highly volatile.Water insoluble, be dissolved in ethanol and ether.Its unstable chemcial property, easy dissociating and discharge nitric oxide gas is prone to oxidized.Can be used as industrial chemicals in the chemical industry field, can be used as the nitric oxide gas donor at medical domain.Laboratory gas chromatographic analysis commonly used detects nitrous ether (ethyl nitrite) gas, but owing to lack the nitrous ether (ethyl nitrite) calibrating gas, is difficult to it is carried out quantitative analysis.
For the detection of gas, lacking under the situation of standard items, adopt static distribution method at present usually.Static distribution method adopts clean air as mist usually, and nitrous ether (ethyl nitrite) is when adopting static distribution method, in containing the air of oxygen, is prone to oxidizedly, and the gas that is made into is inaccurate.The method of a small amount of nitrous ether (ethyl nitrite) calibrating gas of prepared in laboratory still belongs to blank at present.
[summary of the invention]
Technical problem to be solved by this invention provides a kind of preparation method of a small amount of nitrous ether (ethyl nitrite) calibrating gas, to produce the nitrous ether (ethyl nitrite) calibrating gas that the laboratory needs more fast and accurately.
According to the preparation method of nitrous ether (ethyl nitrite) calibrating gas provided by the invention, this method may further comprise the steps:
A1, inert gas is put into clean hermetic flexible containers 1;
A2, nitrous ether (ethyl nitrite) standard items liquid is injected in the clean airtight peace bottle with the micro-chromatography sample introduction needle;
A3, will pacify the bottle be placed in the container 2, with the slow eluant container 2 of the inert gas in the flexible container 1, with the air in the emptying container 2;
A4, container 2 is pumped into negative pressure and airtight;
A5, firmly rock container 2, make 150 fragmentations of peace bottle, treat that nitrous ether (ethyl nitrite) volatilizees fully after, container 2 in, continue to replenish nitrogen, behind the interior air pressure and outside atmosphere equilibrium of container 2, once more that container 2 is airtight;
A6, shake container 2 gently, gas is fully mixed, accomplish preparation nitrous ether (ethyl nitrite) calibrating gas.
According to the present invention in one preferred implementation, in step a2, be that the nitrous ether (ethyl nitrite) standard items liquid of 95% 1uL is injected in the peace bottle 150 with purity.
In one preferred implementation, the volume V1 of hermetic flexible containers 1 is greater than the volume V2 of container 2 according to the present invention, and V1 is 3 times of V2.
In one preferred implementation, the concentration of prepared nitrous ether (ethyl nitrite) calibrating gas is C=(95%* ρ * R*T*1uL)/M*V*P according to the present invention, and wherein ρ is 95% nitrous ether (ethyl nitrite) standard items density of liquid; M is the molal weight of 95% nitrous ether (ethyl nitrite) standard items liquid; R is an ideal gas constant; T is 20 ℃ of normal temperature; P is 1 standard atmospheric pressure 101kPa; V is the volume of container 2.
In invention one preferred implementation, inert gas is a high pure nitrogen.
In invention one preferred implementation, hermetic flexible containers 1 is polybag or balloon.
The nitrous ether (ethyl nitrite) calibrating gas purity of producing through the present invention is higher, speed is faster, and it is more convenient to produce mode.Operability is stronger in the laboratory.
[description of drawings]
Fig. 1 is the flow chart of nitrous ether (ethyl nitrite) calibrating gas produced according to the present invention;
Fig. 2 is the sketch map of the equipment of nitrous ether (ethyl nitrite) calibrating gas produced according to the present invention.
[specific embodiment]
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Fig. 1 shows the flow chart that one embodiment of the present invention prepares the nitrous ether (ethyl nitrite) calibrating gas.
Fig. 2 shows the sketch map that the present invention prepares the equipment of nitrous ether (ethyl nitrite) calibrating gas, and according to the present invention, this equipment that is used to prepare the nitrous ether (ethyl nitrite) calibrating gas comprises: hermetic flexible containers 110 is used to deposit inert gas; Closed container 120 uses in process for preparation, and after preparation is accomplished, is used to deposit calibrating gas; Airtight folder 130 is used to control flexible container 110 and container 120 is communicated with; Airtight folder 140 is used to control container 120 and outside being communicated with; Peace bottle 150 is used to deposit a small amount of nitrous ether (ethyl nitrite) liquid; And bottle stopper 160 is used for closed container 120.Wherein, in the present invention, this container 120 is a vial.The volume V1 of used hermetic flexible containers 110 is greater than the volume V2 of closed container 120, and V1 is 3-5 a times of V2, is preferably 4 times.
With reference to figure 1 and Fig. 2, in step 101, airtight folder 130 is opened, in clean flexible container 110, put into inert gas.Preferably, this inert gas is a high pure nitrogen.In other embodiments of the present invention, also can adopt other inert gases.
In step 102, airtight folder 130 and 140 cuts out.
In step 103, nitrous ether (ethyl nitrite) standard items liquid is injected in the clean airtight peace bottle 150 with the micro-chromatography sample introduction needle.In this embodiment, be that 95% 1uL nitrous ether (ethyl nitrite) standard items liquid is injected in the peace bottle 150 with purity, wherein this purity is that 95% nitrous ether (ethyl nitrite) standard items liquid can be bought on market.
In step 104, will pacify bottle 150 and be placed in the container 120.
In step 105, airtight folder 130 and 140 is opened.
In step 106,,, airtight folder 130 cuts out with the air in the emptying container 120 with the slow eluant container 120 of the high pure nitrogen in the flexible container 110.
In step 107, close airtight folder 130, container 120 is pumped into negative pressure and airtight.
In step 108, close airtight folder 140, firmly rock container 120, make peace bottle 150 fragmentations in the container 120.
In step 109, treat that nitrous ether (ethyl nitrite) volatilizees fully after, open airtight folder 130, in container 120, continue to replenish nitrogen.
In step 110, treat the air pressure and outside atmosphere equilibrium in the container 120 after, close airtight folder 130 and 140, once more that container 120 is airtight.For air pressure and the outside atmosphere equilibrium that makes in the container 120, used hermetic flexible containers 110 in the present invention, the volume of this hermetic flexible containers 110 can reach air pressure balance according to the situation variation of container inner and outer air pressure inside and outside container.In the present invention, hermetic flexible containers 110 is polybag or balloon.
In step 111, shake container 120 gently, container 120 interior gases are fully mixed; Promptly accomplished the preparation of nitrous ether (ethyl nitrite) calibrating gas.
The concentration of prepared according to the method for the invention nitrous ether (ethyl nitrite) calibrating gas is C=(95%* ρ * R*T*1uL)/M*V*P; Wherein ρ is that 95% nitrous ether (ethyl nitrite) standard items density of liquid, M are the molal weight of 95% nitrous ether (ethyl nitrite) standard items liquid, and ρ, M producer when the nitrous ether (ethyl nitrite) standard items liquid of buying 95% can indicate; R is an ideal gas constant; T is 20 ℃ of normal temperature; P is 1 standard atmospheric pressure 101kPa; V is the volume of container 120.
The embodiment of the invention is applicable to laboratory normal temperature, the normal pressure a small amount of ppm (10 of configuration down
-6) level nitrous ether (ethyl nitrite) calibrating gas, method is simple for this, and produce gas purity also than higher, and practicality is very strong.Fill up the laboratory and produced the blank in nitrous ether (ethyl nitrite) calibrating gas field, had application value.
In the above-described embodiments, only the present invention has been carried out exemplary description, but those skilled in the art can carry out various modifications to the present invention after reading present patent application under the situation that does not break away from the spirit and scope of the present invention.
Claims (6)
1. the preparation method of a nitrous ether (ethyl nitrite) calibrating gas is characterized in that, said method comprising the steps of:
A1, inert gas is put into clean hermetic flexible containers 1;
A2, nitrous ether (ethyl nitrite) standard items liquid is injected in the clean airtight peace bottle with the micro-chromatography sample introduction needle;
A3, said peace bottle is placed in the closed container 2, with the slow flushing said container 2 of the said inert gas in the said flexible container 1, with the air in the said container 2 of emptying;
A4, said container 2 is pumped into negative pressure and airtight;
A5, firmly rock said container 2; Make that said peace bottle is broken, treat that nitrous ether (ethyl nitrite) volatilizees fully after, continue to replenish said inert gas through 1 pair of said container 2 of hermetic flexible containers; Behind the air pressure and outside atmosphere equilibrium in said container 2, once more that said container 2 is airtight;
A6, shake said container 2 gently, said gas is fully mixed, with preparation nitrous ether (ethyl nitrite) calibrating gas.
2. preparation method according to claim 1 is characterized in that, in step a2, is that the nitrous ether (ethyl nitrite) standard items liquid of 95% 1uL is injected in the said peace bottle with purity.
3. preparation method according to claim 2 is characterized in that, the volume V1 of said hermetic flexible containers 1 is greater than the volume V2 of said container 2, and said V1 is 3 times of V2.
4. preparation method according to claim 3 is characterized in that, concentration C=(95%* ρ * the R*T*1uL)/M*V*P of said prepared nitrous ether (ethyl nitrite) calibrating gas, and wherein ρ is 95% nitrous ether (ethyl nitrite) standard items density of liquid; M is the molal weight of 95% nitrous ether (ethyl nitrite) standard items liquid; R is an ideal gas constant; T is 20 ℃ of normal temperature; P is 1 standard atmospheric pressure 101kPa; V is the volume of container 2.
5. preparation method according to claim 1 is characterized in that, said inert gas is a high pure nitrogen.
6. preparation method according to claim 1 is characterized in that, said hermetic flexible containers 1 is polybag or balloon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106163926A CN102553468A (en) | 2010-12-30 | 2010-12-30 | Preparation method for ethyl nitrite standard air |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106163926A CN102553468A (en) | 2010-12-30 | 2010-12-30 | Preparation method for ethyl nitrite standard air |
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| CN102553468A true CN102553468A (en) | 2012-07-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104511257A (en) * | 2013-09-26 | 2015-04-15 | 中国石油化工股份有限公司 | Sealed tool for standard gas preparation and preparation device comprising same |
| CN105259014A (en) * | 2015-11-04 | 2016-01-20 | 中国汽车技术研究中心 | Measuring method of VOCs solution and preparation method of standard gas |
| CN107913608A (en) * | 2017-11-10 | 2018-04-17 | 中国人民解放军陆军防化学院 | Air distributing device and air distributing method |
| CN112439342A (en) * | 2020-10-27 | 2021-03-05 | 安徽华塑股份有限公司 | Homogenization compounding device in PVC production process |
-
2010
- 2010-12-30 CN CN2010106163926A patent/CN102553468A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 邵建章: "标准气体的配制技术 ", 《消防技术与产品信息》 * |
| 邵建章: "标准气体的配制技术", 《消防技术与产品信息》, no. 02, 28 February 2002 (2002-02-28), pages 41 - 44 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104511257A (en) * | 2013-09-26 | 2015-04-15 | 中国石油化工股份有限公司 | Sealed tool for standard gas preparation and preparation device comprising same |
| CN105259014A (en) * | 2015-11-04 | 2016-01-20 | 中国汽车技术研究中心 | Measuring method of VOCs solution and preparation method of standard gas |
| CN107913608A (en) * | 2017-11-10 | 2018-04-17 | 中国人民解放军陆军防化学院 | Air distributing device and air distributing method |
| CN107913608B (en) * | 2017-11-10 | 2024-01-02 | 中国人民解放军陆军防化学院 | Air distribution device and air distribution method |
| CN112439342A (en) * | 2020-10-27 | 2021-03-05 | 安徽华塑股份有限公司 | Homogenization compounding device in PVC production process |
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Application publication date: 20120711 |