阅读说明：本技术 一种密封式质谱仪 (Sealed mass spectrometer ) 是由 张兆清 刘权卫 房映彤 侯留东 马敬 陈云清 于 2020-12-03 设计创作，主要内容包括：本发明公开一种密封式质谱仪,用于进行放射性样品分析,包括质谱仪本体,还包括手套箱,所述质谱仪本体包括进样系统及离子源、其他部件,所述进样系统及离子源设于所述手套箱内；所述其他部件设于所述手套箱外。本发明不仅可以保证工作人员的辐射安全,还便于操作、维修。(The invention discloses a sealed mass spectrometer which is used for analyzing radioactive samples and comprises a mass spectrometer body and a glove box, wherein the mass spectrometer body comprises a sample introduction system, an ion source and other components, and the sample introduction system and the ion source are arranged in the glove box; the other components are arranged outside the glove box. The invention can not only ensure the radiation safety of the working personnel, but also facilitate the operation and the maintenance.)

1. A sealed mass spectrometer is used for radioactive sample analysis and comprises a mass spectrometer body and is characterized by also comprising a glove box (4), wherein the mass spectrometer body comprises a sample introduction system, an ion source (2) and other components (8),

the sample introduction system and the ion source are arranged in the glove box;

the other components are arranged outside the glove box.

2. The sealed mass spectrometer according to claim 1, wherein the mass spectrometer body further comprises an interface structure (1), the sample introduction system and the ion source being connected to the other components via the interface structure,

the interface structure comprises a sample cone, a cutting cone and a connecting piece,

the sample cone and the intercepting cone are arranged in the glove box and are opposite to the ion source;

the connecting piece wraps outside the sample cone and the intercepting cone and is in sealing connection with the glove box through a flange.

3. The sealed mass spectrometer of claim 1, wherein the sample introduction system and the ion source are high frequency inductively coupled plasma.

4. The sealed mass spectrometer of claim 1, wherein a slide assembly is provided within the glove box for sliding the sample introduction system and the ion source within the glove box.

5. The sealed mass spectrometer according to claim 4, characterized in that the sliding assembly comprises a carriage, a slide rail (5),

the bracket is arranged below the sample injection system and the ion source, the slide rail is arranged on the bracket along the horizontal direction, and the lower parts of the sample injection system and the ion source are arranged on the slide rail in a penetrating way.

6. Sealed mass spectrometer according to claim 1, characterised in that the further components comprise an exhaust system and a vacuum system, the exhaust system comprising an exhaust tube (9) and an exhaust hood (3),

one end of the exhaust pipe is communicated with the outlet end of a vacuum pump in the vacuum system, and the other end of the exhaust pipe extends into the glove box and is used for introducing gas generated by the vacuum system into the glove box;

the exhaust hood is arranged in the glove box, is positioned near the sample introduction system and the ion source and is used for collecting waste gas generated when the ion source performs plasma treatment on the radioactive sample.

7. The sealed mass spectrometer of claim 1, further comprising a filter assembly,

the filtering component comprises an exhaust filter (6) which is arranged outside the glove box and used for filtering waste gas inside the glove box and discharging the waste gas to the outside of the glove box.

8. The sealed mass spectrometer of claim 7, wherein the filter assembly further comprises an intake air filter,

the air inlet filter is arranged outside the glove box and used for filtering the outside air and then introducing the outside air into the glove box.

9. Sealed mass spectrometer according to one of claims 1-8, characterized in that the glove box comprises a box provided with a plurality of gloves (7),

the box body comprises a plurality of panels, wherein two oppositely arranged panels are made of transparent glass, and other panels are made of stainless steel.

10. The sealed mass spectrometer of claim 9, wherein the glove box further comprises a feedthrough connector, an electrical connector, and a negative pressure monitoring device,

the pipe penetrating joint is used for conveying a reagent;

the electric connector is used for supplying power;

the negative pressure monitoring device is used for monitoring the pressure in the glove box;

and the sealing grade of the glove box is at least 3 grades.

Technical Field

The invention belongs to the technical field of nuclei, and particularly relates to a sealed mass spectrometer for radioactive sample analysis.

Background

Nuclear facilities such as nuclear fuel reprocessing plants and radiochemical test facilities generally need to perform sample analysis, thereby providing necessary parameters for processes such as process flow, product indexes, environmental emission and the like. However, because these samples are radioactive, the pretreatment, analysis, etc. of the samples must be performed in a shielded chamber with a sealing function to ensure the radiation safety of the staff.

The mass spectrometer is a common device for analyzing trace elements, ultra-trace elements and isotopes, in particular to an inductively coupled plasma mass spectrometer (ICP-MS), has the advantages of high precision, accurate measurement, high speed, wide linear range, high resolution and the like, and is an essential means for analyzing samples in nuclear facilities.

However, there is no sealed mass spectrometer specially designed for radioactive sample analysis in the mass spectrometers on the market at present, and when the mass spectrometer is used for analyzing radioactive samples in the past, the whole mass spectrometer needs to be sealed in a customized glove box or a fume hood, so that the operation and maintenance are inconvenient, and the glove box has the characteristics of continuous air intake and exhaust and open operation, so that the problems of instability, easy corrosion, inconvenient maintenance, difficult solid waste treatment and the like exist, and the risk of radioactive escape exists when the mass spectrometer is placed in the fume hood, and the radiation safety of personnel cannot be ensured.

Disclosure of Invention

The invention aims to solve the technical problem of providing a sealed mass spectrometer aiming at the defects in the prior art, which can ensure the radiation safety of workers and is convenient to operate and maintain.

The technical scheme adopted for solving the technical problem of the invention is as follows:

the invention provides a sealed mass spectrometer, comprising:

a sealed mass spectrometer is used for radioactive sample analysis and comprises a mass spectrometer body and a glove box, wherein the mass spectrometer body comprises a sample introduction system, an ion source and other components,

the sample introduction system and the ion source are arranged in the glove box;

the other components are arranged outside the glove box.

Preferably, the mass spectrometer body further comprises an interface structure, the sample introduction system and the ion source are connected with other components through the interface structure, the interface structure comprises a sample cone, a cutting cone and a connecting piece, and the sample cone and the cutting cone are arranged in the glove box and are opposite to the ion source; the connecting piece wraps outside the sample cone and the intercepting cone and is in sealing connection with the glove box through a flange.

Preferably, in the sample introduction system and the ion source, the ion source is a high-frequency inductively coupled plasma.

Preferably, a sliding assembly is arranged in the glove box and used for driving the sample introduction system and the ion source to slide in the glove box.

Preferably, the sliding assembly comprises a bracket and a slide rail, the bracket is arranged below the sampling system and the ion source, the slide rail is arranged on the bracket along the horizontal direction, and the lower parts of the sampling system and the ion source are arranged on the slide rail in a penetrating way.

Preferably, the other components comprise an exhaust system and a vacuum system, the exhaust system comprises an exhaust pipe and an exhaust hood, one end of the exhaust pipe is communicated with an outlet end of a vacuum pump in the vacuum system, and the other end of the exhaust pipe extends into the glove box and is used for introducing gas generated by the vacuum system into the glove box;

the exhaust hood is arranged in the glove box, is positioned near the sample introduction system and the ion source and is used for collecting waste gas generated when the ion source performs plasma treatment on the radioactive sample.

Preferably, the mass spectrometer further comprises a filter assembly, wherein the filter assembly comprises an exhaust filter, and the exhaust filter is arranged outside the glove box and used for filtering and discharging the waste gas inside the glove box to the outside of the glove box.

Preferably, the filter assembly further comprises an air inlet filter, wherein the air inlet filter is arranged outside the glove box and used for filtering the outside air and then introducing the outside air into the glove box.

Preferably, the glove box comprises a box body, a plurality of gloves are arranged on the box body, the box body comprises a plurality of panels, two panels which are oppositely arranged are made of transparent glass, and other panels are made of stainless steel.

Preferably, the glove box further comprises a pipe penetrating joint, an electric connector and a negative pressure monitoring device, wherein the pipe penetrating joint is used for conveying a reagent;

the electric connector is used for supplying power;

the negative pressure monitoring device is used for monitoring the pressure in the glove box;

and the sealing grade of the glove box is at least 3 grades.

The sealed mass spectrometer of the invention has the advantages that the parts needing to be directly contacted with the radioactive sample, such as the feeding system, the ion source and the like, are arranged in the sealed glove box, so that the parts are completely isolated from other parts which are not directly contacted with the radioactive sample.

Drawings

Fig. 1 is a schematic structural diagram of a sealed mass spectrometer according to an embodiment of the present invention.

In the figure: 1-an interface structure; 2-sample introduction system and ion source; 3-an exhaust hood; 4-glove box; 5-a slide rail; 6-an exhaust filter; 7-gloves; 8-other components; 9-exhaust pipe.

Detailed Description

In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflicting with each other.

In the description of the present invention, it is to be understood that the directional terms as used herein are used in a specific orientation or positional relationship shown in the drawings, and are used for convenience in describing the present invention and for simplicity in description, but do not indicate or imply that the device or element so referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be considered as limiting the present invention.

Example 1

As shown in fig. 1, the present embodiment discloses a sealed mass spectrometer including a mass spectrometer body, and a glove box 4, wherein: the mass spectrometer body includes sampling system and ion source 2, other parts 8, and sampling system and ion source 2 locate glove box 4 in, and other parts 8 locate outside glove box 4.

Compare in current mass spectrograph, this embodiment sealed mass spectrograph separates through the part that needs direct contact radioactive sample such as charge-in system and ion source 2 with other parts 8 of the not direct contact radioactive sample in the mass spectrograph body, make both be in the inside and outside of glove box 4 respectively, make and directly carry out preliminary treatment in glove box 4 when carrying out radioactive sample analysis, operations such as feeding, both can prevent that radioactive substance from leaking, ensure staff's radiation safety, and convenient operation, be convenient for maintain, and do not change mass spectrometer's analysis performance parameter.

In some embodiments, the mass spectrometer body further includes an interface structure 1, the interface structure 1 is disposed on the glove box 4, and the sample introduction system and the ion source 2 are connected to other components 8 through the interface structure 1. Specifically, the other components 8 include ion lenses, mass analyzers, detectors, and other components, the interface structure 1 includes sample cones, skimmer cones, and connectors, and the glove box includes a box body, wherein the sample cones and skimmer cones (having the same or similar composition as that of the existing mass spectrometer) are disposed in the glove box 4, and the sample cones are opposite to the ion source, so as to suck ions generated during plasma processing at the ion source, and transmit the sucked ions into cavities of the subsequent components such as ion lenses, mass analyzers, and detectors in the other components 8 in the mass spectrometer body; the connecting piece parcel passes through flange sealing connection outside sample awl and intercepting awl, and with the box of glove box 4, and the sample awl can avoid radioactive substance to leak.

In some embodiments, the ion source employs a high frequency inductively coupled plasma and the mass spectrometer body is an inductively coupled plasma mass spectrometer. More specifically, the inductively coupled plasma mass spectrometer can be an inductively coupled plasma mass spectrometer (ICP-MS) with a mass analyzer of a quadrupole, a high resolution mass spectrometer (HR-ICP-MS) with a mass analyzer of electromagnetic double focusing, a multi-receiver mass spectrometer (MC-ICP-MS), and other mass spectrometers with similar related structures and easy sealing.

In some embodiments, a sliding assembly is disposed in the glove box 4 for driving the sample feeding system and the ion source 2 to slide in the glove box 4, so that the feeding system and the ion source 2 are located at positions convenient for the operation and maintenance of the worker, and after the operation and maintenance are completed, the feeding system and the ion source 2 are slid to the original position.

In some embodiments, the slide assembly comprises a carriage, a slide rail 5 (or a slide bar). The bracket is arranged below the sample introduction system and the ion source 2 and has an adjusting function, for example, the bottom of the bracket can be provided with a horizontal adjusting screw rod to adjust the horizontal position of the bracket, and the bottom of the bracket can also be provided with a vertical adjusting screw rod to adjust the height of the bracket. The slide rail 5 is arranged on the bracket along the horizontal direction, and the lower parts of the feeding system and the ion source 2 are arranged on the slide rail 5 in a penetrating way.

In some embodiments, the sliding assembly further comprises a power member and a control switch (not shown), wherein the power member is connected with the feeding system and the ion source 2 to provide the moving power, and the control switch is electrically connected with the power member to control the power member to output the power. The control switch is preferably provided outside the glove box 4, for example, on a side panel of the box body of the glove box 4.

In some embodiments, the power member may be an electric cylinder, i.e. the feeding system and the ion source 2 are driven to move by electric power, and the electric cylinder is controlled to be electrified by a control switch. The power part can also be a cylinder, namely, the feeding system and the ion source 2 are driven to move by adopting a pneumatic mode, and air is fed into the cylinder by controlling a control switch.

In some embodiments, the glove box 4 may be sized to: the length is 1200-1200 mm, the width is 800-1200mm, and the height is 1400-2000mm, so as to ensure that the glove box 4 has a large enough inner space to meet the requirements of operation, maintenance and the like. In this embodiment, a plurality of gloves 7 are arranged on the box body of the glove box 4, the box body comprises a plurality of panels, specifically, the box body comprises a plurality of side plates, a top plate at the upper part and a bottom plate at the lower part, the gloves 7 are preferably arranged on two opposite side plates in the box body of the glove box 4, the number of the gloves 7 can be selected according to requirements, for example, 6-10 gloves can be respectively arranged, and the two opposite side plates provided with the gloves 7 are preferably made of transparent glass, for example, transparent organic glass or toughened glass. The feeding cone in the interface structure 1 is arranged on any one of the rest side plates in the box body, and the side plate, the top plate, the bottom plate and the rest side plates are preferably made of stainless steel.

In some embodiments, the other components 8 of the sealed mass spectrometer of this embodiment include an exhaust system and a vacuum system, the exhaust system includes an exhaust pipe 9 and an exhaust hood 3, and the vacuum system includes a vacuum pump, wherein one end of the exhaust pipe 9 is communicated with an outlet end of the vacuum pump in the vacuum system, and the other end thereof extends into the glove box 4 for introducing exhaust gas generated by the vacuum system into the glove box 4; the exhaust hood 3 is disposed in the glove box 4 and near the sample injection system and the ion source, for example, may be disposed right above the sample injection system and the ion source, and is configured to collect exhaust gas generated when the ion source performs plasma processing on the radioactive sample. The waste gas generated by the vacuum system and the waste gas generated by the plasma treatment are collected into the glove box 4 to be treated and discharged in a unified way, so that the radioactive substances can be prevented from leaking, the pollution to the working environment is prevented, and the operation is convenient.

In some embodiments, the sealed mass spectrometer of the present embodiment further includes a filter assembly including a vent filter 6, the vent filter 6 is disposed outside the glove box 4, for example, on the ceiling of the glove box 4, an end of the vent pipe 9 extending into the glove box 4 is located at an inlet of the vent filter 6, and the vent filter 6 is preferably also located above or at an outlet of the exhaust hood 3, so as to filter and exhaust the exhaust gas inside the glove box 4 (including the exhaust gas exhausted by the vacuum system and the exhaust gas generated at the ion source) to the outside of the glove box 4.

In some embodiments, the filter assembly further comprises an intake filter disposed outside the glove box 4, for example, on a ceiling of the glove box 4, for filtering and passing ambient air into the glove box 4 to help regulate and maintain the pressure within the glove box 4.

In some embodiments, the glove box 4 is further provided with a negative pressure monitoring device (not shown in the figures), which is used for detecting the pressure inside the glove box 4 and ensuring that the pressure inside the glove box 4 is maintained at a required negative pressure to prevent the radioactive substance from leaking. In this embodiment, the negative pressure value in the glove box 4 is preferably-200 to-300 Pa.

In some embodiments, the glove box 4 may further include a tube connector, an electrical connector, and a lamp (not shown) and other auxiliary components, which may be selected according to actual requirements, wherein the tube connector is used for conveying a reagent, the electrical connector is used for supplying power, and the lamp is used for lighting.

In some embodiments, the sealed mass spectrometer of the present embodiment may further include a support, and the mass spectrometer body and the glove box 4 are both disposed on the support, and the height of the support is preferably 500 mm and 800mm, so as to be conveniently operated by a worker.

In some embodiments, the glove box 4 should have a sealing rating of at least 3 to ensure sealing effectiveness.

In summary, in the sealed mass spectrometer of the present embodiment, the components such as the feeding system and the ion source that need to directly contact the radioactive sample are disposed in the sealed glove box, so as to be completely isolated from the components such as the ion lens, the mass analyzer, the detector, and the vacuum system that do not directly contact the radioactive sample in the mass spectrometer body.

It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.