CN106769243A - A kind of amine sampling pipe and preparation method thereof and its application method - Google Patents
A kind of amine sampling pipe and preparation method thereof and its application method Download PDFInfo
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- CN106769243A CN106769243A CN201611176466.2A CN201611176466A CN106769243A CN 106769243 A CN106769243 A CN 106769243A CN 201611176466 A CN201611176466 A CN 201611176466A CN 106769243 A CN106769243 A CN 106769243A
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- amine
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2273—Atmospheric sampling
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- General Health & Medical Sciences (AREA)
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- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to the technical field of organic amine material sampling, more particularly, to a kind of amine sampling pipe and preparation method thereof and its application method.A kind of amine sampling pipe, wherein, including glass tube, filling glass cotton in glass tube, the both ends of glass tube are provided with closure after sampling.This sampling pipe of the invention can gather more volatile organic amines, improve sampling efficiency, and analyzing efficiency, subsequent treatment is simple and easy to carry.
Description
Technical field
The present invention relates to the technical field of organic amine material sampling, more particularly, to a kind of amine sampling pipe and its system
Make method and its application method.
Background technology
In the car, in track traffic and indoor and surrounding air, organic amine material is the allusion quotation for being only second to organic sulfur compound
Type odorant pollutant, has irritation, do harm to huamn body to eye, nose, throat.Sampling pipe common at present, absorbing liquid is only
For dimethylamine, trimethylamine, such as oxalic acid-glass microballoon sampling pipe, neutral silica gel pipe, its mesoxalic acid-glass microballoon sampling pipe has
Effect phase only one of which month, laboratory parsing, com-parison and analysis are cumbersome after sampling, are unfavorable for large batch of sample analysis, experimental result
Stability be difficult to ensure that；Absorbing liquid can solve sampling efficiency and parsing efficiency（Need not parse）But, absorbing liquid
Carry transport inconvenient.
In the prior art, the sampling of oxalic acid glass microballoon is fairly simple, but cumbersome, the batch processing difficulty of post processing is tested after sampling
Greatly, the degree of accuracy and poor reproducibility are tested；Fibers adsorption pipe and silica gel absorption pipe absorption dimethylamine and trimethylamine utilize physical absorption,
It is with strong points；Absorb liquid energy and improve adsorption efficiency, but absorbing liquid is unfavorable for storing and transports.Auto parts and components, track traffic and
There are fatty amines, aromatic amine, other amines etc. to be not limited to dimethylamine and trimethylamine in surrounding air.
The content of the invention
The present invention is to overcome at least one defect described in above-mentioned prior art, there is provided a kind of amine sampling pipe and its making side
Method and its application method, can gather more volatile organic amines, improve sampling efficiency and analyzing efficiency, subsequent treatment it is simple and
It is easy to carry.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of amine sampling pipe, wherein, including glass
Pipe, filling glass cotton in glass tube, the both ends of glass tube are provided with closure after sampling.
In the present invention, including：Blank pipe, pretreated mineral wool, closure；Blank pipe makes for glass, and mineral wool is through phosphorus
Low-kappa number mistake, sampling pipe is that the pretreated mineral wool of certain mass is filled in glass tube, high-temperature digestion two ends glass
Sealing preserve, the sampling pipe being made.
Further, described glass tube includes glass tube main body, the glass tube leading section located at glass tube main body one end.
Described glass tube main body is shaped as cylindrical shape.Being shaped as described glass tube leading section is coniform.Glass tube main body master
Play a part of carrying, the inside is equipped with pretreated mineral wool.The diameter of glass tube leading section is gradually reduced, glass tube front end
The shape in portion is similar to as coniform.
Further, described glass tube main body is provided with screens, described mineral wool with the junction of glass tube leading section
One end be connected in screens.In the present invention, screens is the structure of a projection, can block mineral wool, prevents it in sampling pipe
It is mobile.In addition, in order to block mineral wool, may be alternatively provided as other interface arrangments, above-mentioned interface arrangment is of the invention
In protection domain.
Further, the end of described glass tube main body is provided with the first cutting mouth, and described glass tube front end sets
There is the second cutting mouth.During sampling, opened from the first cutting mouth, the second cutting mouth, gas flow direction is the second cutting mouth end
Enter, the first cutting mouth brings out, after completing sampling, preserved after sampling pipe two end cap top cover labyrinth.
The preparation method of described amine sampling pipe, wherein：Comprise the following steps：
S1. put mineral wool into round-bottomed flask, add phosphoric acid acetonitrile solution, be spin-dried for using Rotary Evaporators；
S2. the mineral wool that 0.05g soaked is weighed to enter in glass tube；
S3. high-temperature digestion two ends glass capsulation, preserves at 0-8 °C.
In described step S1, phosphoric acid acetonitrile solution is 200ml0.2%；Using Rotary Evaporators, in 43 °C of 100r/min
Under conditions of be spin-dried for.
Preparation method：Put mineral wool into round-bottomed flask, add the phosphoric acid acetonitrile solution of 200ml0.2%, use rotation
Turn evaporimeter, be spin-dried under conditions of 43 °C of 100r/min.It is accurate to weigh the mineral wool that 0.05g soaked and enter in glass tube, it is high
Temperature dissolving two ends glass capsulation, 0-8 °C of preservation.The mineral wool that 0.05g soaked can be adapted to the requirement of glass tube size.
The application method of described amine sampling pipe, wherein：Comprise the following steps：
S10. the first cutting mouth of cutting sampling pipe and the second cutting mouth end, connect the first cutting mouth end and adopt using silicone tube
Sample pump is sampled, and air enters sampling pipe by the second cutting mouth end；
S20. add formic acid+methyl alcohol+water to enter sampling pipe, elute repeatedly, detected with liquid phase second order mses, calculate the concentration of amine.
In step S10, sample rate is 50ml/min ~ 6000ml/min, sampling time 60min；Described step S20
In, 2ml formic acid+methyl alcohol+water is added, ratio is 0.02:1:1 (V/V) enters sampling pipe, elutes 3 to 4 times repeatedly.
Sampling pipe sampling flow rates：50ml/min ~ 6000ml/min, can meet the sampling of low middle high flow rate.
Compared with prior art, beneficial effect is：This sampling pipe of the invention can gather more volatile organic amines, and raising is adopted
Sample efficiency, analyzing efficiency, subsequent treatment is simple and easy to carry.
Brief description of the drawings
Fig. 1 is overall structure diagram of the present invention.
Fig. 2 is amine mixed standard solution table of the present invention.
Specific embodiment
Accompanying drawing being for illustration only property explanation, it is impossible to be interpreted as the limitation to this patent；It is attached in order to more preferably illustrate the present embodiment
Scheme some parts to have omission, zoom in or out, do not represent the size of actual product；To those skilled in the art,
Some known features and its explanation may be omitted and will be understood by accompanying drawing.Being for illustration only property of position relationship described in accompanying drawing
Explanation, it is impossible to be interpreted as the limitation to this patent.
As shown in figure 1, a kind of amine sampling pipe, wherein, including glass tube 1, filling glass cotton 2 in glass tube 1, glass after sampling
The both ends of glass pipe 1 are provided with closure 14.
In the present embodiment, including：Blank pipe, pretreated mineral wool 2, closure 14；Blank pipe makes for glass, mineral wool 2
It is pretreated through phosphoric acid, sampling pipe is that the pretreated mineral wool of certain mass is filled in glass tube 1, high-temperature digestion two
End glass capsulation is preserved, the sampling pipe being made.
Glass tube 1 includes glass tube main body 100, the glass tube leading section 200 located at the one end of glass tube main body 100.Glass
Pipe main body 100 is shaped as cylindrical shape.Being shaped as glass tube leading section 200 is coniform.
Glass tube main body 100 primarily serves the effect of carrying, and the inside is equipped with pretreated mineral wool 2.Glass tube leading section
200 diameter is gradually reduced, and the shape of glass tube leading section is similar to as coniform.
In the present embodiment, glass tube main body 100 is provided with screens 13 with the junction of glass tube leading section 200, mineral wool 2
One end is connected in screens 13.In the present embodiment, screens 13 is the structure of a projection, can block mineral wool 2, prevents it in sampling
In-pipe.In addition, in order to block mineral wool, may be alternatively provided as other interface arrangments, above-mentioned interface arrangment is in this hair
In bright protection domain.
The end of glass tube main body 100 is provided with the first cutting mouth 11, and the second cutting mouth is provided with glass tube leading section 200
12。
As shown in the figure：A kind of amine sampling pipe, including glass tube 1, through the pretreated mineral wool 2 of phosphoric acid, by certain mass
Pretreated mineral wool 2 be filled in glass tube, filling position at screens 13, high-temperature digestion two ends glass capsulation preserve,
The sampling pipe being made.Operation instruction：During sampling, opened from the first cutting mouth of cutting mouth 11, the second cutting mouth 12, gas stream
To enter at the end of the second cutting mouth 12, the first cutting mouth 11 brings out in dynamic direction, after completing sampling, after sampling pipe two end cap top cover labyrinth 14
Preserve.
Mineral wool is a kind of manmade inorganic fibre.The natural crystals such as quartz sand, lime stone, dolomite are used for main former
Material, under melting state, cotton-shaped fine fibre is got rid of into by external force blowing produced, is crossings on different level between fiber and fiber, is twined mutually
Around many tiny holes, are showed together, huge surface area is produced, mineral wool after pretreatment can be by phosphoric acid solution
Absorption.Easily adsorbed by phosphoric acid absorbing liquid when organic amine gas in air are by mineral wool.
Specifically, preparation method：Put mineral wool into round-bottomed flask, add the phosphoric acid acetonitrile solution of 200ml0.2%,
Using Rotary Evaporators, it is spin-dried under conditions of 43 °C of 100r/min.It is accurate to weigh the mineral wool that 0.05g soaked and enter glass
In pipe, high-temperature digestion two ends glass capsulation, 0-8 °C of preservation.
Application method：Cutting sampling pipe 11 and 12 end, connects 11 ends and sampling pump is sampled using silicone tube, air by
12 ends enter sampling pipe, sample rate 1000ml/min, sampling time 60min.Add 2ml formic acid+methyl alcohol+water (0.02:1:1)
(V/V) enter sampling pipe, elute 3 to 4 times repeatedly, use liquid phase second order mses（LC-MS/MS）Detection, calculates the concentration of amine.
Sampling flow velocity：Sampling pipe sampling flow rates：50ml/min ~ 6000ml/min, can meet adopting for low middle high flow rate
Sample.
Experiment shows, with mineral wool as absorbing liquid carrier, be crossings on different level between microglass fiber and fiber, mutually
Be intertwined, show many tiny holes, produce huge surface area, the amine in air by when be easy to by surface
Absorbing liquid absorption.Eluted using 2ml oxalic acid methanol aqueous solutions, substantially without amine residual on glass wool material.It is quantitative to add
Enter containing 0.6 μ g amine mixed standard solutions（Fig. 2 is specifically shown in, organic amine includes but is not limited to following species）To in sampling pipe, pass through
1000mL/min high pure nitrogens, simulated air sampling process.The various amine rate of recovery >=90%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not right
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.There is no need and unable to be exhaustive to all of implementation method.It is all this
Any modification, equivalent and improvement made within the spirit and principle of invention etc., should be included in the claims in the present invention
Protection domain within.
Claims (10)
1. a kind of amine sampling pipe, it is characterised in that including glass tube（1）, glass tube（1）Interior filling glass cotton（2）, glass after sampling
Glass pipe（1）Both ends be provided with closure（14）.
2. a kind of amine sampling pipe according to claim 1, it is characterised in that：Described glass tube（1）Including glass tube master
Body（100）, located at glass tube main body（100）The glass tube leading section of one end（200）.
3. a kind of amine sampling pipe according to claim 2, it is characterised in that：Described glass tube main body（100）With glass
Pipe leading section（200）Junction be provided with screens（13）, described mineral wool（2）One end be connected in screens（13）On.
4. a kind of amine sampling pipe according to claim 3, it is characterised in that：Described glass tube main body（100）End
It is provided with the first cutting mouth（11）, described glass tube leading section（200）Place is provided with the second cutting mouth（12）.
5. according to a kind of any described amine sampling pipes of claim 2-4, it is characterised in that：Described glass tube main body（100）
Be shaped as cylindrical shape.
6. according to a kind of any described amine sampling pipes of claim 2-4, it is characterised in that：Described glass tube leading section
（200）Be shaped as it is coniform.
7. the preparation method of the amine sampling pipe described in claim 6, it is characterised in that：Comprise the following steps：
S1. put mineral wool into round-bottomed flask, add phosphoric acid acetonitrile solution, be spin-dried for using Rotary Evaporators；
S2. the mineral wool that 0.05g soaked is weighed to enter in glass tube；
S3. high-temperature digestion two ends glass capsulation, preserves at 0-8 °C.
8. the preparation method of amine sampling pipe according to claim 7, it is characterised in that：In described step S1, phosphoric acid second
Nitrile solution is 200ml0.2%；Using Rotary Evaporators, it is spin-dried under conditions of 43 °C of 100r/min.
9. the application method of the amine sampling pipe described in claim 6, it is characterised in that：Comprise the following steps：
S10. the first cutting mouth of sampling pipe is cut（11）With the second cutting mouth（12）End, connects first and cuts using silicone tube
Mouthful（11）End and sampling pump are sampled, and air is by the second cutting mouth（12）End enters sampling pipe；
S20. add formic acid+methyl alcohol+water to enter sampling pipe, elute repeatedly, detected with liquid phase second order mses, calculate the concentration of amine.
10. the application method of amine sampling pipe according to claim 9, it is characterised in that：In described step S10, sampling
Speed is 50ml/min ~ 6000ml/min, sampling time 60min；In described step S20,2ml formic acid+methyl alcohol+water is added,
Ratio is 0.02:1:1 (V/V) enters sampling pipe, elutes 3 to 4 times repeatedly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611176466.2A CN106769243B (en) | 2016-12-19 | 2016-12-19 | Amine sampling tube, manufacturing method and using method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611176466.2A CN106769243B (en) | 2016-12-19 | 2016-12-19 | Amine sampling tube, manufacturing method and using method thereof |
Publications (2)
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| CN106769243A true CN106769243A (en) | 2017-05-31 |
| CN106769243B CN106769243B (en) | 2023-05-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107621392A (en) * | 2017-11-16 | 2018-01-23 | 中国烟草总公司郑州烟草研究院 | Gas phase nicotine separates harvester and its method with grain phase nicotine in a kind of aerosol |
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| CN106769243B (en) | 2023-05-16 |
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