WO2020253239A1 - 一种进样装置 - Google Patents

一种进样装置 Download PDF

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Publication number
WO2020253239A1
WO2020253239A1 PCT/CN2020/072430 CN2020072430W WO2020253239A1 WO 2020253239 A1 WO2020253239 A1 WO 2020253239A1 CN 2020072430 W CN2020072430 W CN 2020072430W WO 2020253239 A1 WO2020253239 A1 WO 2020253239A1
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Prior art keywords
sample
moving part
transfer
cavity
transfer chamber
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PCT/CN2020/072430
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English (en)
French (fr)
Inventor
龚冰
郑永飞
Original Assignee
中国科学技术大学
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Application filed by 中国科学技术大学 filed Critical 中国科学技术大学
Priority to DE112020001039.2T priority Critical patent/DE112020001039T5/de
Publication of WO2020253239A1 publication Critical patent/WO2020253239A1/zh
Priority to US17/485,847 priority patent/US11699581B2/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0409—Sample holders or containers
    • H01J49/0413—Sample holders or containers for automated handling
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/04—Details of the conveyor system
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0422—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for gaseous samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/04—Details of the conveyor system
    • G01N2035/0439—Rotary sample carriers, i.e. carousels
    • G01N2035/0441—Rotary sample carriers, i.e. carousels for samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/04—Details of the conveyor system
    • G01N2035/046—General conveyor features
    • G01N2035/0465—Loading or unloading the conveyor
    • 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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G01N30/7206—Mass spectrometers interfaced to gas chromatograph

Definitions

  • the invention relates to the technical field of analytical instruments, in particular to a sampling device.
  • the sampling device In the pretreatment of elemental analysis and isotope analysis, the sampling device has a great influence on the accuracy and accuracy of the analysis. Therefore, a reasonably designed and efficient sampling device can be used to analyze the element content and isotope composition of the sample. Important.
  • the sample In the work of using the element analyzer to analyze the elements of the sample, the sample is usually directly dropped from the sample pan into the element analyzer.
  • the sample is pre-processed by high-temperature baking before the analysis, the adsorption on the sample surface Air and a small amount of moisture in the atmosphere are difficult to remove completely, especially powder samples are greatly affected.
  • the impurities (ie, air and moisture) adsorbed on the surface of these samples will directly affect the background of the sample analysis. For some samples with low element content, it will seriously affect the accuracy and sensitivity of the analysis.
  • the present invention provides a sample injection device that can work with an analyzer to significantly improve the accuracy and sensitivity of sample analysis.
  • the present invention provides the following technical solutions:
  • a sampling device including:
  • a processing system arranged on the body and capable of purging and vacuuming the samples in the transfer chamber with helium gas.
  • the moving member is a moving rod provided in the inner cavity of the body, and axially reciprocates in the inner cavity.
  • the body is provided with a sample exit hole, the sample exit hole is located at the bottom of the moving part, and the sample can enter from the transfer cavity through the sample exit hole.
  • the sample exit hole is located at the bottom of the moving part, and the sample can enter from the transfer cavity through the sample exit hole.
  • the transfer cavity is opened along the radial direction of the moving part and penetrates the moving part, so that the sample on the sample tray moves to the sample injection position in the transfer cavity It can fall into the transfer cavity, and the sample in the transfer cavity can fall into the sample outlet hole when the transfer cavity moves to the sample outlet position.
  • the processing system includes a helium gas pipeline, an evacuation pipeline, and a solenoid valve.
  • the transfer chamber moves to the processing position, the helium pipeline and the evacuation pipeline are connected to the The transfer chambers are alternately communicated, and the solenoid valve is respectively communicated with the vacuum pipe and the helium pipe through a vacuum interface and a helium interface to control the on and off of the vacuum pipe and the helium pipe.
  • the processing position is located between the sample injection position and the sample discharge position.
  • a plurality of sealing rings are sleeved on the moving part, and all the sealing rings are sealingly connected to the outer circumferential wall of the moving part and the inner wall of the inner cavity, and are respectively located in the Both sides of the transfer cavity are kept tightly closed when the transfer cavity is in communication with the helium gas pipeline and the vacuum pipeline.
  • the sample tray is rotatably arranged on the body, and a first compressed air inlet is provided on the body, and the compressed air entering from the first compressed air inlet is used for driving The sample pan rotates.
  • a second compressed air inlet is provided on the body, and the compressed air entering from the second compressed air inlet is used to drive the moving part to move back and forth.
  • a vacuum gauge is provided in the transfer chamber.
  • the sample injection device provided by the present invention can realize automatic sample injection through the relay transport of the sample tray and the moving part to the sample, and in the process of transporting the sample by the moving part, the helium purging of the sample can be realized through the processing system And vacuuming, so as to remove the air adsorbed by the sample through helium purging, and remove the moisture adsorbed by the sample through vacuuming, thereby minimizing the background of the analysis, and significantly improving the accuracy and sensitivity of elemental analysis and isotope analysis.
  • Figure 1 is a schematic structural diagram of a sample injection device provided by an embodiment of the invention.
  • the invention provides a sample injection device, which can work with an analyzer to significantly improve the accuracy and sensitivity of sample analysis.
  • an embodiment of the present invention provides a sample injection device, which is used to work with an analyzer.
  • the sample injection device mainly includes: a body 11; a sample tray 1 arranged on the body 11, and the sample tray 1 Used to temporarily place the weighed sample to be analyzed; a moving part 2 that is set on the body 11 and can reciprocate on the body 11, and the moving part 2 is provided with a transfer cavity 6 that can receive the sample tray 1
  • the sample sent can be transferred to the analyzer with the movement of the moving part 2 to realize the transportation of the sample to the analyzer; it is set on the body 11 and can perform helium gas on the sample in the transfer chamber 6 Purge and vacuum processing system.
  • the above-mentioned sample injection device can purify and vacuum the sample in the transfer chamber 6 with helium gas through the processing system during the sample transportation process, thereby removing impurities such as air and moisture adsorbed by the sample, allowing the sample element analysis and analysis The accuracy and sensitivity of isotope analysis can be greatly improved.
  • the moving part 2 is a moving rod arranged in the inner cavity of the body 11 and moves axially back and forth in the inner cavity. Choosing the moving part 2 as a rod-shaped part and placing it inside the body 11 not only simplifies the structure of the sampling device and reduces its volume, but it can also be realized more easily through the cooperation of the inner cavity and the moving rod.
  • the transfer chamber 6 is sealed, so this structure is regarded as the preferred structure of this embodiment.
  • the moving part 2 may also be arranged outside the body 11.
  • the body 11 is provided with a sample outlet 3, and preferably the sample outlet 3 is located at the bottom of the moving part 2, and the sample can enter the reaction tube of the analyzer from the transfer chamber 6 through the sample outlet 3 .
  • the structure where the sample enters the analyzer from the sample injection device is preferably a sample outlet 3 opened on the body 11 and capable of communicating with the transfer chamber 6 (in addition, it can also be set specifically to communicate with the transfer chamber 6 and the analysis
  • This structure can simplify the overall structure of the sample injection device, and make the sample outlet 3 located at the bottom of the moving part 2. It can also make the transfer chamber 6 communicate with the sample outlet 3 when the sample is under its own weight. It is directly dropped into the reaction tube under the action of, so there is no need to set up special driving parts, so as to reduce the manufacturing cost of the sampling device and improve the working performance.
  • the transfer cavity 6 is opened along the radial direction of the moving part 2 and penetrates the moving part 2, so that the sample on the sample tray 1 moves to the sample injection position in the transfer chamber 6 (ie, the index in Figure 1 When there is a position C), it can fall into the transfer chamber 6, and the sample in the transfer chamber 6 can fall into the sample exit hole when the transfer chamber 6 moves to the sample exit position (ie the position marked A in Figure 1) 3 in.
  • Opening the transfer cavity 6 along the radial direction of the moving part 2 facilitates the cooperation of the moving part 2 with the sample tray 1 at its top and the sample outlet 3 at the bottom, that is, through the moving part 2 during the sample transportation process
  • the transfer chamber 6 moves to the sample injection position
  • the transfer chamber 6 is aligned with the sample tray 1, so the sample on the sample tray 1 can fall directly into the transfer chamber from the top entrance of the transfer chamber 6 Within 6.
  • the bottom outlet of the transfer chamber 6 is aligned with and communicated with the sample outlet 3, and the sample in the transfer chamber 6 can directly fall into the sample outlet through the bottom outlet In hole 3, and finally into the reaction tube of the analyzer.
  • the preferred processing system includes a helium gas pipeline, an evacuation pipeline, and a solenoid valve 7.
  • the solenoid valve 7 is connected to the vacuum pipe and the helium pipe through the vacuum interface 4 and the helium interface 5 respectively to control the on and off of the vacuum pipe and the helium pipe, and the helium pipe is connected with a high-purity helium source to pump A vacuum dry pump is connected to the vacuum pipeline.
  • the transfer chamber 6 will first move to the sample processing position (ie The position marked B in Figure 1), so that the helium pipe and the vacuum pipe can communicate with the transfer chamber 6 to perform sample processing on the sample in the transfer chamber 6.
  • the sample processing position ie The position marked B in Figure 1
  • the solenoid valve 7 It is connected with the transfer chamber 6, so that helium purging of the sample is realized by introducing helium into the transfer chamber 6.
  • the helium gas pipeline is disconnected by the solenoid valve 7, and then the solenoid valve 7 controls the vacuum pipeline It is connected to the transfer chamber 6, and the transfer chamber 6 is evacuated under the vacuum action of the vacuum dry pump to remove the air in the transfer chamber 6 and the gas (including air and water vapor) adsorbed on the sample surface, and then the solenoid valve 7 Disconnect the vacuum line.
  • the helium purging and vacuuming are performed alternately 4-6 times, and the vacuum degree in the transfer chamber 6 is detected by a vacuum gauge. When the vacuum degree reaches 10 -2 -10 -3 mbar, it can basically be considered that the air adsorbed on the sample surface and After the water treatment is completed, the treatment operation is completed. Afterwards, the sample with impurities removed moves to the sample output position and enters the sample output hole 3.
  • the processing position is preferably located between the sample injection position and the sample output position.
  • This arrangement enables the sample in the transfer chamber 6 to pass through the processing position during the process of approaching the sample discharge position, avoiding the increase in the moving distance of the moving part 2 due to the processing position being set on the same side of the sample injection position and the sample discharge position. Large, so that the working performance of the sampling device can be improved.
  • a plurality of sealing rings 8 are sleeved on the moving part 2. As shown in FIG. 1, all the sealing rings 8 are sealingly connecting the outer circumferential wall of the moving part 2 and the inner wall of the inner cavity of the body 1, and They are respectively located on both sides of the transfer chamber 6 so that the transfer chamber 6 is kept airtight when communicating with the helium gas pipeline and the vacuum pipeline. Since it is necessary to ensure the sealing of the transfer chamber 6 when processing the samples in the transfer chamber 6, a sealing ring 8 is provided between the outer circumferential wall of the moving part 2 and the inner wall of the inner cavity of the body 11. The sealing ring 8 seals the transfer chamber.
  • the cavity 6 becomes a closed space when it is not located at the sampling position and the sampling position, which ensures the smooth progress of helium purging and vacuuming.
  • the sealing of the transfer cavity 6 can also be achieved in other ways, for example, a sealed door that can be opened and closed is provided at the top entrance and the bottom exit of the transfer cavity 6.
  • the sample tray 1 is rotatably arranged on the body 11, and the body 11 is also provided with a first compressed air inlet 9, and the compressed air entering from the first compressed air inlet 9 is used to drive the sample tray 1 rotates, and at the same time, the body 11 is provided with a second compressed air inlet 10, and the compressed air entering from the second compressed air inlet 10 is used to drive the moving part 2 to move back and forth.
  • the reciprocating movement of the movable member 2 and the rotation of the sample plate 1 are preferably realized by the driving of compressed air.
  • the movement of the moving part 2 and the sample tray 1 can also be driven by other types of driving methods, such as motors, air cylinders, hydraulic cylinders and other components.
  • a vacuum gauge is preferably provided in the transfer chamber 6, so that the sample processing can be monitored by the vacuum gauge, so that the background of analysis can be minimized.
  • the status of sample processing can also be obtained through other monitoring methods, such as setting up a vacuum gauge and a flow meter on the vacuum pipeline.
  • the bake temperature can be adjusted higher, generally 150 ⁇ -200 ⁇ , and the bake time is 24 hours.
  • the bake temperature is normal. Set 80 ⁇ -120 ⁇ , the baking time is 12 hours; then accurately weigh the sample and wrap it in a high-purity tin cup, place the weighed sample in sample tray 1; rotate sample tray 1, and the sample falls into the Transfer chamber 6 at the sample position; after the transfer chamber 6 moves to the processing position, under the control of the solenoid valve 7, the sample is alternately purged and evacuated with helium gas; using a vacuum gauge, when the vacuum degree of the transfer chamber 6 reaches At 10 to 2 mbar, it can be considered that the impurities adsorbed by the sample are basically removed; then the transfer chamber 6 moves to the sample output position, and the sample falls into the oxidation-reduction reaction tube under the helium atmosphere for reaction; the tail gas is separated by the GC column, according to The amount of carbon dioxide can get the content of
  • the sample When analyzing the water content and H isotope composition in minerals, the sample is first baked. For water-containing minerals, the baking temperature is 100 ⁇ -120 ⁇ , and the baking time is 6 hours. For minerals that are nominally anhydrous (that is, the molecular formula does not contain water) ) Mineral, the baking temperature is 120 ⁇ -150 ⁇ , and the baking time is 8 hours; then the sample is accurately weighed and wrapped in a high-purity silver cup, the weighed sample is placed in the sample pan 1; the sample pan 1 is rotated , The sample falls into the transfer chamber 6 at the sample injection position. Since the water adsorbed on the sample surface is difficult to remove, the temperature in the transfer chamber 6 needs to be set to 100 ⁇ ; then the transfer chamber 6 is moved to the processing position.
  • the samples are purged and evacuated alternately with helium. Because the water adsorbed on the sample surface is difficult to remove, it takes a long time to purify and evacuate the sample with helium; use a vacuum gauge when the degree of vacuum transfer chamber 6 reaches 10-2 mbar, the sample can be considered substantially removing adsorbed impurities; then moved to the transfer chamber 6 the sample position, sample falls carbon reduction furnace under helium environment; tail gas by GC The column is separated and then enters the isotope gas mass spectrometer. According to the peak area of hydrogen, the mineral water content and H isotope composition can be calculated.
  • sample injection device provided in this embodiment has the following advantages compared with the traditional sample injection device:
  • each part is described in a progressive manner.
  • the structure of each part focuses on the difference from the existing structure.
  • the entire and partial structure of the sampling device can be combined with the above-mentioned multiple parts. And get.

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Abstract

本申请公开了一种进样装置，包括：机体；设置在机体上的样品盘；设置在机体上，并能在机体上往复移动的移动件，且移动件上开设有转移腔，转移腔能接收样品盘送来的样品，并能随着移动件的移动将样品转移至分析仪中；设置在机体上，并能对位于转移腔中的样品进行氦气吹扫和抽真空的处理系统。上述的进样装置，通过样品盘和移动件对样品的接力运送，能够实现样品的自动进样，并且在移动件运送样品的过程中，能够通过处理系统实现对样品的氦气吹扫和抽真空，从而通过氦气吹扫将样品表面吸附物(空气和水等)剥离，通过抽真空将剥离的样品表面吸附物(空气和水等)去除，进而最大限度的降低分析的本底，显著提高元素分析和同位素分析的精度和灵敏度。

Description

一种进样装置
本申请要求于2019年6月21日提交中国专利局、申请号为201910542627.2、发明名称为“一种进样装置”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及分析仪器技术领域，特别涉及一种进样装置。
背景技术
在元素分析和同位素分析的预处理中，进样装置对于分析的精度和准确度的影响极大，因此，一个设计合理、高效的进样装置在分析样品的元素含量和同位素组成的工作中至关重要。
在利用元素分析仪对样品进行元素分析的工作中，样品一般是直接由样品盘落入到元素分析仪中，尽管在分析之前对样品进行了高温烘烤等预处理，但是样品表面所吸附的空气和少量大气中的水气很难去除完全，尤其是粉末样品受到的影响较大。这些样品表面吸附的杂质(即空气和水分)会直接影响样品分析的本底，对于一些元素含量低的样品，会严重影响分析的精度和灵敏度。
发明内容
有鉴于此，本发明提供了一种进样装置，令其与分析仪配合工作，能够显著提升对样品进行分析的精度和灵敏度。
为了达到上述目的，本发明提供如下技术方案：
一种进样装置，包括：
机体；
设置在所述机体上的样品盘；
设置在所述机体上，并能够在所述机体上往复移动的移动件，且所述移动件上开设有转移腔，所述转移腔能够接收所述样品盘送来的样品，并能够随着所述移动件的移动将所述样品转移至分析仪中；
设置在所述机体上，并能够对位于所述转移腔中的所述样品进行氦气吹扫和抽真空的处理系统。
优选的，上述进样装置中，所述移动件为设置在所述机体的内腔中的移动杆，并在所述内腔中轴向往复移动。
优选的，上述进样装置中，所述机体上开设有出样孔，所述出样孔位于所述移动件的底部，且所述样品能够通过所述出样孔从所述转移腔进入到所述分析仪的反应管中。
优选的，上述进样装置中，所述转移腔沿所述移动件的径向开设并贯通所述移动件，以使所述样品盘上的所述样品在所述转移腔移动至进样位置时能够落入到所述转移腔中，并使所述转移腔中的所述样品在所述转移腔移动至出样位置时能够落入到所述出样孔中。
优选的，上述进样装置中，所述处理系统包括氦气管道、抽真空管道和电磁阀，在所述转移腔移动至处理位置时，所述氦气管道和所述抽真空管道与所述转移腔交替连通，所述电磁阀通过真空接口和氦气接口分别与所述抽真空管道和所述氦气管道连通，以控制所述抽真空管道和所述氦气管道的通断。
优选的，上述进样装置中，在所述移动件的轴向上，所述处理位置位于所述进样位置和所述出样位置之间。
优选的，上述进样装置中，所述移动件上套设有多个密封圈，全部所述密封圈均密封连接所述移动件的圆周外壁和所述内腔的内壁，并分别位于所述转移腔的两侧，以使所述转移腔在与所述氦气管道和所述抽真空管道连通时保持密闭。
优选的，上述进样装置中，所述样品盘转动的设置在所述机体上，且所述机体上设置有第一压缩空气进口，从所述第一压缩空气进口进入的压缩空气用于驱动所述样品盘转动。
优选的，上述进样装置中，所述机体上设置有第二压缩空气进口，从所述第二压缩空气进口进入的压缩空气用于驱动所述移动件往复移动。
优选的，上述进样装置中，所述转移腔内设置有真空计。
本发明提供的进样装置，通过样品盘和移动件对样品的接力运送，能够实现样品的自动进样，并且在移动件运送样品的过程中，能够通过处理系统实现对样品的氦气吹扫和抽真空，从而通过氦气吹扫将样品吸附的空气去除，通过抽真空将样品吸附的水分去除，进而最大限度的降低分析的本底，显著提高元素分析和同位素分析的精度和灵敏度。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图获得其他的附图。
图1为本发明实施例提供的进样装置的结构示意图。
在图1中：
1-样品盘，2-移动件，3-出样孔，4-真空接口，5-氦气接口，6-转移腔，7-电磁阀，8-密封圈，9-第一压缩空气进口，10-第二压缩空气进口，11-机体。
具体实施方式
本发明提供了一种进样装置，令其与分析仪配合工作，能够显著提升对样品进行分析的精度和灵敏度。
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
如图1所示，本发明实施例提供了一种进样装置，其用于配合分析仪工作，该进样装置主要包括：机体11；设置在机体11上的样品盘1，此样品盘1用于临时放置称量好的待分析样品；设置在机体11上，并能够在机体11上往复移动的移动件2，且移动件2上开设有转移腔6，转移腔6能够接收样品盘1送来的样品，并能够随着移动件2的移动将样品转移至分析仪中，以实现样品向分析仪的运送；设置在机体11上，并能够对位于转移腔6中的样品进行氦气吹扫和抽真空的处理系统。
上述的进样装置，能够在样品运送的过程中，通过处理系统对位于转移腔6内的样品进行氦气吹扫和抽真空，从而去除样品吸附的空气和水分等杂质，令样品元素分析和同位素分析的精度和灵敏度能够得到大幅提升。
为了进一步优化技术方案，本实施例提供的进样装置中，如图1所示，移动件2为设置在机体11的内腔中的移动杆，并在内腔中轴向往复移动。选用移动件2为杆状件，并将其设置在机体11的内部，不仅能够简化进样装置的结构，令其体积得以减小，而且还能够通过内腔和移动杆的配合更容易的实现 转移腔6的密闭，所以将此种结构作为本实施例的优选结构。此外，在保证正常工作的前提下，移动件2也可以设置在机体11的外部。
如图1所示，机体11上开设有出样孔3，并优选该出样孔3位于移动件2的底部，且样品能够通过出样孔3从转移腔6进入到分析仪的反应管中。本实施例中，样品从进样装置进入到分析仪的结构，优选为开设在机体11上并能够与转移腔6连通的出样孔3(此外也可以设置专门用于连通转移腔6和分析仪反应管的输送管)，此结构能够简化进样装置的整体结构，并且令出样孔3位于移动件2的底部，还可以使转移腔6在与出样孔3连通时令样品在自身重量的作用下直接落入到反应管中，从而无需设置专门的驱动部件，以降低进样装置的制造成本，提升工作性能。
如图1所示，本实施例还优选转移腔6沿移动件2的径向开设并贯通移动件2，以使样品盘1上的样品在转移腔6移动至进样位置(即图1中标有C的位置)时能够落入到转移腔6中，并使转移腔6中的样品在转移腔6移动至出样位置(即图1中标有A的位置)时能够落入到出样孔3中。将转移腔6沿移动件2的径向开设，有利于移动件2与位于其顶部的样品盘1以及位于其底部的出样孔3进行配合，即在样品输送的过程中，通过移动件2的移动使转移腔6移动至进样位置时，由于此时的转移腔6与样品盘1对正，所以能够使得样品盘1上的样品能够从转移腔6的顶部入口直接落入到转移腔6内。当移动件2通过移动使转移腔6移动至出样位置时，转移腔6的底部出口与出样孔3对正且连通，转移腔6内的样品就可以通过底部出口直接落入到出样孔3中，并最终进入到分析仪的反应管中。
本实施例中，优选处理系统包括氦气管道、抽真空管道和电磁阀7，如图1所示，在转移腔6移动至处理位置时，氦气管道和抽真空管道与转移腔6交替连通，电磁阀7通过真空接口4和氦气接口5分别与抽真空管道和氦气管道连通，以控制抽真空管道和氦气管道的通断，并且氦气管道外接有高纯氦气源，抽真空管道外接有真空干泵。当转移腔6移动至进样位置承接样品后，移动件2会带动位于转移腔6中的样品向出样位置移动，在此移动的过程中，转移腔6会先移动至样品处理位置(即图1中标有B的位置)，从而使得氦气管道和抽真空管道能够与转移腔6连通而对转移腔6中的样品进行样品处理，在进行 处理时，先通过电磁阀7令氦气管道与转移腔6连通，从而通过将氦气导入到转移腔6中实现对样品的氦气吹扫，吹扫完成后再通过电磁阀7将氦气管道断开，然后电磁阀7控制抽真空管道与转移腔6连通，在真空干泵的真空作用下对转移腔6进行抽真空，以将转移腔6内的空气和样品表面所吸附的气体(包括空气和水气)去除，之后令电磁阀7断开抽真空管路。上述氦气吹扫和抽真空交替进行4-6次，并通过真空计检测转移腔6内真空度，当真空度达到10 -2-10 -3mbar时，基本可以认为样品表面吸附的空气和水处理完毕，处理操作完成。之后去除杂质的样品移动至出样位置并进入出样孔3。
如图1所示，在移动件2的轴向上，优选处理位置位于进样位置和出样位置之间。如此设置，能够使得转移腔6内的样品在向出样位置靠近的过程中就经过处理位置，避免因处理位置设置在进样位置和出样位置的同一侧而使移动件2的移动距离增大，从而可以令进样装置的工作性能得到提升。
进一步的，本实施例还优选移动件2上套设有多个密封圈8，如图1所示，全部密封圈8均密封连接移动件2的圆周外壁和机体1的内腔的内壁，并分别位于转移腔6的两侧，以使转移腔6在与氦气管道和抽真空管道连通时保持密闭。由于在对转移腔6内的样品进行处理时需要保证转移腔6的密闭，所以在移动件2的圆周外壁和机体11内腔的内壁之间设置密封圈8，通过密封圈8的密封使转移腔6在不位于进样位置和出样位置时成为密闭空间，保证氦气吹扫和抽真空的顺利进行。此外，转移腔6的密闭，还可以通过其他方式实现，例如在转移腔6的顶部入口和底部出口处均设置能够开闭的密封门等。此外，本实施例中，优选密封圈8为三个，如图1所示。
具体的，如图1所示，样品盘1转动的设置在机体11上，且机体11上还设置有第一压缩空气进口9，从第一压缩空气进口9进入的压缩空气用于驱动样品盘1转动，同时，机体11上设置有第二压缩空气进口10，从第二压缩空气进口10进入的压缩空气用于驱动移动件2往复移动。即，本实施例中移动件2的往复移动以及样品盘1的转动，均优选通过压缩空气的驱动而实现。此外，移动件2和样品盘1的运动，还可以通过其他类型的驱动方式实现驱动，例如通过电机、气缸、液压缸等部件进行驱动。
本实施例中，优选在转移腔6内设置有真空计，以使样品处理的情况可以 通过真空计进行监控，从而可以最大限度降低分析的本底。此外，样品处理的情况也可以通过其他监测方式而得到，例如在抽真空管路上设置真空计、流量计等。
下面分别以分析矿物中碳元素含量和分析矿物中水含量及其同位素组成为例来说明进样装置的具体工作过程：
在分析矿物中碳元素含量时，首先烘烤样品，对于无机样品，可以将烘烤温度适当调高，一般为150□-200□，烘烤时间为24小时，对于有机样品，烘烤温度一般设为80□-120□，烘烤时间为12小时；随后准确称量样品并包裹于高纯锡杯中，将称量好的样品放置于样品盘1中；样品盘1转动，样品落入位于进样位置的转移腔6中；转移腔6之后移动至处理位置，此时在电磁阀7控制下，交替对样品进行氦气吹扫和抽真空；利用真空计，当转移腔6的真空度达到10- 2毫巴时，可以认为样品吸附的杂质基本去除；然后转移腔6移动至出样位置，样品落入氦气环境下的氧化-还原反应管中进行反应；尾气通过GC柱分离，根据二氧化碳的量，可以得到矿物中碳元素的含量。
在分析矿物中水含量和H同位素组成时，首先烘烤样品，对于含水矿物，烘烤温度为100□-120□，烘烤时间为6小时，对于名义上无水的矿物(即分子式不含水)矿物，烘烤温度为120□-150□，烘烤时间为8小时；随后准确称量样品并包裹于高纯银杯中，将称量好的样品放置于样品盘1中；样品盘1转动，样品落入位于进样位置的转移腔6中，由于样品表面吸附的水很难去除，因此需要将转移腔6内的温度设为100□；之后令转移腔6移动至处理位置，此时在电磁阀7控制下，交替对样品进行氦气吹扫和抽真空，由于样品表面吸附的水比较难以去除，因此，对样品进行氦气吹扫和抽真空的时间需要较长；利用真空计，当转移腔6真空度达到10- 2毫巴时，可以认为样品吸附的杂质基本去除；然后转移腔6移动至出样位置，样品落入氦气环境下的碳还原炉中；尾气通过GC柱分离，再进入同位素气体质谱仪中，根据氢气的峰面积可以计算出矿物水含量及H同位素组成。
综上，本实施例提供的进样装置与传统进样装置相比具备以下优势：
(1)更高的分析精度。通过进样前对样品的氦气吹扫和抽真空，基本去除吸附杂质对分析的影响，相较于传统操作方法，分析精度可以提高一个数量 级；
(2)更高分析灵敏度。传统操作方法对于极低含量的样品，由于吸附杂质的影响，往往无法测量，本实施例提供的进样装置能够成功实现零本底，极大地提高了分析灵敏度。
本说明书中对各部分结构采用递进的方式描述，每个部分的结构重点说明的都是与现有结构的不同之处，进样装置的整体及部分结构可通过组合上述多个部分的结构而得到。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (10)

  1. 一种进样装置，其特征在于，包括：
    机体；
    设置在所述机体上的样品盘；
    设置在所述机体上，并能够在所述机体上往复移动的移动件，且所述移动件上开设有转移腔，所述转移腔能够接收所述样品盘送来的样品，并能够随着所述移动件的移动将所述样品转移至分析仪中；
    设置在所述机体上，并能够对位于所述转移腔中的所述样品进行氦气吹扫和抽真空的处理系统。
  2. 根据权利要求1所述的进样装置，其特征在于，所述移动件为设置在所述机体的内腔中的移动杆，并在所述内腔中轴向往复移动。
  3. 根据权利要求2所述的进样装置，其特征在于，所述机体上开设有出样孔，所述出样孔位于所述移动件的底部，且所述样品能够通过所述出样孔从所述转移腔进入到所述分析仪的反应管中。
  4. 根据权利要求3所述的进样装置，其特征在于，所述转移腔沿所述移动件的径向开设并贯通所述移动件，以使所述样品盘上的所述样品在所述转移腔移动至进样位置时能够落入到所述转移腔中，并使所述转移腔中的所述样品在所述转移腔移动至出样位置时能够落入到所述出样孔中。
  5. 根据权利要求4所述的进样装置，其特征在于，所述处理系统包括氦气管道、抽真空管道和电磁阀，在所述转移腔移动至处理位置时，所述氦气管道和所述抽真空管道与所述转移腔交替连通，所述电磁阀通过真空接口和氦气接口分别与所述抽真空管道和所述氦气管道连通，以控制所述抽真空管道和所述氦气管道的通断。
  6. 根据权利要求5所述的进样装置，其特征在于，在所述移动件的轴向上，所述处理位置位于所述进样位置和所述出样位置之间。
  7. 根据权利要求5所述的进样装置，其特征在于，所述移动件上套设有多个密封圈，全部所述密封圈均密封连接所述移动件的圆周外壁和所述内腔的内壁，并分别位于所述转移腔的两侧，以使所述转移腔在与所述氦气管道和所 述抽真空管道连通时保持密闭。
  8. 根据权利要求2-7中任意一项所述的进样装置，其特征在于，所述样品盘转动的设置在所述机体上，且所述机体上设置有第一压缩空气进口，从所述第一压缩空气进口进入的压缩空气用于驱动所述样品盘转动。
  9. 根据权利要求2-7中任意一项所述的进样装置，其特征在于，所述机体上设置有第二压缩空气进口，从所述第二压缩空气进口进入的压缩空气用于驱动所述移动件往复移动。
  10. 根据权利要求1-7中任意一项所述的进样装置，其特征在于，所述转移腔内设置有真空计。
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CN102636659A (zh) * 2012-05-09 2012-08-15 长沙瑞翔科技有限公司 自动进样装置
DE202015004524U1 (de) * 2015-06-24 2016-09-29 C. Gerhardt GmbH & Co. KG Analyseeinrichtung für die Elementaranalyse
CN105403613A (zh) * 2015-10-23 2016-03-16 中国科学技术大学 真空分步加热-元素-同位素富集分析装置
CN205620426U (zh) * 2016-05-04 2016-10-05 中国科学院寒区旱区环境与工程研究所 元素分析仪和固体自动进样器在线连接使用的漏检排查帽
CN109557226A (zh) * 2018-12-04 2019-04-02 中国科学院地质与地球物理研究所 一种用于测定氮同位素的进样系统及其进样方法
CN110164748A (zh) * 2019-06-21 2019-08-23 中国科学技术大学 一种进样装置
CN210006693U (zh) * 2019-06-21 2020-01-31 中国科学技术大学 一种进样装置

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