CN104730177A - Enrichment apparatus used for collecting a variety of pollutants in high vacuum environment and use method thereof - Google Patents

Abstract

The invention discloses a concentrator for collecting various pollutants in a high-vacuum environment and a use method thereof. The concentrator includes an adsorption material placed inside the concentrator; the concentrator includes a shell body The inner cavity structure composed of the shell cover and the cover on it, the adsorption material is placed in the inner cavity, a number of non-straight-through holes are distributed around the wall of the shell body, and multiple concentrators are hung or Put it in the appropriate position of the vacuum system, and the adsorption material absorbs the volatiles generated by the detection system. On the one hand, the present invention reduces the influence of optical and magnetic effects that may exist in the vacuum system on the adsorption material; on the other hand, it can prevent the leakage of the adsorption material in the vacuum environment and avoid polluting the environment.

Description

Concentrator for collection of multiple pollutants in high vacuum environment and method of use

technical field

The invention relates to a chemical substance sampling and enriching device dispersed in space in a high vacuum environment, and is a novel vacuum sample sampling and enriching device and a use method thereof.

Background technique

In recent years, the aerospace industry has developed rapidly, and the ascension of the ten gods marks that my country's aerospace industry has entered a new era. Aerospace engineering equipment usually needs to be applied in a vacuum environment. The existence of some particles, inorganic and organic pollutants in the vacuum may have adverse effects on the devices and engineering projects in the vacuum environment. Therefore, the collection of pollutants in the vacuum, Detection to determine its composition, source, and distribution in vacuum is helpful for contamination source determination and pollution control. The collection and measurement technology of pollutants in vacuum environment is the premise of carrying out related research.

At present, the common method of vacuum sampling is to place a stainless steel plate or quartz plate as a receiving plate in the vacuum device, take it out after a period of time, wipe the pollutants with quartz wool soaked in solvent, then soak the quartz wool with solvent, and take the solution for analysis. Due to the bulky collection device and the limited area for receiving pollutants in this method, the collection efficiency of pollutants is not high, which affects the detection sensitivity and accuracy.

For the analysis of gaseous volatiles with low content, it usually needs to be enriched and concentrated to reach the detection limit of the instrument in order to achieve accurate determination. Enrichment and concentration methods include active sampling and passive sampling. The active sampling method is to absorb or retain a large number of gaseous samples through the absorption liquid or solid absorbent, so that the pollutants with a small concentration can be concentrated, which is convenient for analysis and determination, but an air pump is required, which is difficult to achieve in a high-vacuum environment ; The passive sampling method uses a diffuse mechanism, that is, molecular pollutants diffuse to the sampler by natural diffusion. Passive adsorption mainly relies on the interaction of intermolecular forces including dispersion force, induction force and orientation force for adsorption. This method combines the advantages of better sensitivity, simplicity and practicality, and more reasonable equipment prices.

The passive sampling method can use the solid-phase adsorption method. Due to the special vacuum environment, placing the adsorption material directly in the vacuum environment for static adsorption is easy to contaminate the vacuum equipment.

Contents of the invention

Purpose of the invention: In order to overcome the deficiencies in the prior art, the present invention provides a concentrator for collecting various pollutants in a high-vacuum environment and its use method, on the one hand, it can reduce the optical, magnetic, etc. that may exist in the vacuum system. Effect on the adsorption material, on the other hand, it can block the leakage of the adsorption material in the vacuum environment and avoid polluting the environment.

Technical scheme: in order to achieve the above object, the technical scheme adopted in the present invention is:

A concentrator for collecting various pollutants in a high vacuum environment, including a concentrator and an adsorption material arranged inside the concentrator; the concentrator consists of a shell body and a shell cover covering it Inner cavity structure, the adsorption material is placed in the inner cavity, and a number of non-through holes are distributed around the wall of the shell body.

Further, the non-straight-through hole is a curved and irregularly shaped hole that runs through the wall of the housing body, and the size of the hole is 50 μm.

Further, the adsorption material is a clean porous material or an electrospun nanofiber material.

Further, the shape of the electrospun nanofiber material is adjusted through raw material composition, voltage, temperature and humidity, so as to realize the collection of pollutants in a broad spectrum range.

The method for using the concentrator for collecting multiple pollutants in a high vacuum environment, the specific steps are as follows:

1) Place or hang multiple concentrators at appropriate positions in the vacuum system according to the needs of the actual situation;

2) With the vacuuming operation of the vacuum system, the volatiles generated by the vacuum system will be adsorbed in the adsorption material in the enricher;

3) When detection is required, the adsorption material is taken out of the concentrator, eluted with a small amount of solvent for analysis or headspace thermal analysis, and the obtained analysis solution or analysis gas is injected into the detection instrument for detection.

Further, put the taken-out adsorption material in a stoppered test tube, add 0.4ml of methanol to soak for 2 hours, take the methanol solution and inject it into GC-MC for detection and analysis, and obtain the content and type information of organic pollutants; the adsorption material after soaking in methanol solution The material was blown dry with a nitrogen blower under the condition of a constant temperature water bath at 50°C, and eluted with 500 μL of 5% (V/V) HNO ₃ . The eluate was transferred to a centrifuge tube. The volume of %HNO ₃ was adjusted to 2ml, and detected by ICP-MS to obtain the pollution of metal elements.

Beneficial effect: advantage of the present invention:

1. The concentrator of the present invention is made of sintered stainless steel powder, and is a metal material containing curved and irregularly shaped non-straight-through holes. On the one hand, these non-straight-through holes can ensure that gaseous pollutants at the molecular level can pass freely The concentrator shell is adsorbed by the adsorption material, which prevents external radiation and light from reaching the adsorption material; on the other hand, it also prevents the small particle pollutants of the adsorption material from escaping into the vacuum environment to further pollute the vacuum equipment.

2. In the present invention, after the adsorption material is taken out from the concentrator, a small amount of solvent is used for elution analysis or headspace thermal analysis, and the obtained analysis liquid or analysis gas is injected into the detection instrument for detection, and organic pollutants and inorganic pollutants can be obtained type and content information.

Description of drawings

Fig. 1 is a sectional view of the internal structure of the concentrator of the present invention.

Fig. 2 is a schematic structural diagram of the concentrator of the present invention.

Fig. 3 is a schematic diagram of the structure of the concentrator of the present invention placed or suspended inside the vacuum system.

Fig. 4 is a blank chromatogram-mass detection spectrum of the methanol solvent of the present invention.

Fig. 5 is a blank chromatogram-mass spectrum detection spectrum for methanol elution of the adsorption material of the present invention.

Fig. 6 is a chromatographic-mass spectrogram of the methanol eluent of the adsorption material when there is a pollution source in the vacuum system cabin of the present invention.

Fig. 7 is a schematic diagram of the types and contents of metal elements adsorbed by the adsorption material of the present invention.

Detailed ways

The present invention will be further described below in conjunction with the accompanying drawings.

The purpose of the present invention is to solve the difficult problem of sampling pollutants in the vacuum environment and overcome the deficiencies of the traditional vacuum sampling technology.

As shown in accompanying drawings 1 and 2, it is a concentrator for collecting various pollutants in a high vacuum environment, including a concentrator 3 and an adsorption material arranged inside the concentrator 3; the concentrator 3 includes a shell The inner cavity structure composed of the shell body 2 and the shell cover 1 covering it, the adsorption material is placed in the inner cavity, and a number of non-through holes 5 are distributed around the wall surface of the shell body 2 .

The non-straight-through hole 5 is a curved and irregularly shaped hole and is arranged through the wall of the shell body 2 , and the size of the hole is 50 μm.

The adsorption material is a clean porous material or an electrospun nanofiber material. The present invention uses electrospun nanofibers as the adsorption material (disclosed in utility model 201120291026.8). The diameter of the material is nanometer or submicron size, and the length is micrometer, millimeter or even longer. It has high-efficiency adsorption characteristics and better operability than nanometer fiber particles and other nanomaterials. By changing the type of nanofibers and adjusting the shape of the electrospun nanofiber material through raw material composition, voltage, temperature and humidity, the collection of pollutants in a broad spectrum range can be realized, and the fabrication is simple and easy for industrialization.

In order to cooperate with the present invention, a plastic film with dibutyl phthalate as a plasticizer is selected as the pollution source 6 and placed in the vacuum system cabin to investigate the adsorption effect of the concentrator on vacuum pollutants.

The method of using the concentrator for collecting various pollutants in a high-vacuum environment, firstly, according to the needs of the experiment, use electrospinning technology to prepare nanofiber materials with different chemical compositions. different. The diameter and shape of the electrospun nanofiber material in the present invention can be adjusted by controlling the spinning conditions such as raw material composition, voltage, temperature and humidity. The spun electrospun nanofiber material is purified and weighed quantitatively, placed in the shell body 2 of the concentrator 3 , and the shell cover 1 of the concentrator 3 is covered to form the concentrator 3 . Specific steps are as follows:

1) As shown in the accompanying drawing 3, place or suspend a plurality of concentrators 3 made in the proper position of the vacuum system;

2) With the vacuuming operation of the vacuum system, the volatile matter produced by the vacuum system will be adsorbed in the adsorption material in the enricher 3;

3) When detection is required, the adsorption material is taken out from the concentrator 3, eluted with a small amount of solvent for analysis or headspace thermal analysis, and the obtained analysis solution or analysis gas is injected into the detection instrument for detection.

Specifically, for the above step 3), put the taken-out adsorbent material into a stoppered test tube, add 0.4ml of methanol to soak for 2 hours, take the methanol solution and inject it into GC-MS for detection and analysis, and obtain the organic pollution situation; after soaking in methanol solution The adsorbent material was blown dry with a nitrogen blowing instrument under the condition of a constant temperature water bath at 50°C, and eluted with 5% (V/V) HNO ₃ 500 μL, and the eluate was transferred to a centrifuge tube, and after a total of three elutions, the eluate Dilute to 2ml with 5% HNO ₃ , and detect with ICP-MS to obtain metal element pollution.

As shown in accompanying drawings 4, 5 and 6, the present invention obtains organic matter dibutyl phthalate through GC-MC detection and analysis, indicating that the concentrator 3 has a better adsorption effect on organic pollutants. As shown in accompanying drawing 7, the adsorption material of concentrator 3 detects more Na, Ca, Al, As, Zn etc. by ICP-MS, detects less metal elements such as Ni, Cu, and draws the conclusion When there is a plastic film, more metal elements are diffused into the vacuum, and the results show that the concentrator 3 of the present invention also has a better trapping effect on metal elements.

The above is only a preferred embodiment of the present invention, it should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications are also possible. It should be regarded as the protection scope of the present invention.

Claims (6)

1. for the enricher that multiple pollutant in high vacuum environment gathers, it is characterized in that: comprise enricher (3) and be arranged on the inner sorbing material of enricher (3); Described enricher (3) comprises the internal cavity structure that shell body (2) and lid casing cover (1) thereon form, described sorbing material is placed in internal cavity, and the wall surrounding of described shell body (2) is distributed with some non-through-type holes (5).

2. according to claim 1 for the enricher of multiple pollutant collection in high vacuum environment, it is characterized in that: described non-through-type hole (5) is bending erose hole and runs through the wall setting of shell body (2), and the size of hole is 50 μm.

3. according to claim 1 for the enricher that multiple pollutant in high vacuum environment gathers, it is characterized in that: described sorbing material is clean porosint or electro spinning nano fiber material.

4. according to claim 3 for the enricher that multiple pollutant in high vacuum environment gathers, it is characterized in that: the shape being adjusted described electro spinning nano fiber material by raw material composition, voltage, temperature and humidity, realizes the collection of wide spectrum range contamination thing.

5., for the using method of the enricher of multiple pollutant collection in high vacuum environment, it is characterized in that, concrete steps are as follows:

1) according to actual conditions need the suitable position of vacuum system is put or hung on to multiple enricher (3);

2) along with vacuum system vacuumizes operation, the volatile matter that vacuum system produces will be adsorbed in the sorbing material in enricher (3);

3) when needs detect, taken out by sorbing material from enricher (3), resolve or head space Thermal desorption with a small amount of solvent elution, the desorbed solution obtained or resolution gas inject detecting instrument and detect.

6. according to claim 5 for the using method of the enricher of multiple pollutant collection in high vacuum environment, it is characterized in that: the sorbing material of taking-up is placed in tool plug test tube, add 0.4ml methyl alcohol and soak 2 hours, get methanol solution and inject GC-MC detection analysis, obtain organic contaminant content and kind of information; Sorbing material after methanol solution soaks is dried up with Nitrogen evaporator under 50 DEG C of water bath with thermostatic control conditions, with 5% (V/V) HNO ₃500 μ L wash-outs, eluent goes in centrifuge tube, after co-elute three times, by eluent 5%HNO ₃be settled to 2ml, detect with ICP-MS, obtain metal element content and kind of information.