WO2017113625A1 - 多通道顶空提取针 - Google Patents

多通道顶空提取针 Download PDF

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Publication number
WO2017113625A1
WO2017113625A1 PCT/CN2016/085695 CN2016085695W WO2017113625A1 WO 2017113625 A1 WO2017113625 A1 WO 2017113625A1 CN 2016085695 W CN2016085695 W CN 2016085695W WO 2017113625 A1 WO2017113625 A1 WO 2017113625A1
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Prior art keywords
tube
needle tube
needle
pipeline
sample
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PCT/CN2016/085695
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English (en)
French (fr)
Inventor
何启发
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成都科林分析技术有限公司
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Application filed by 成都科林分析技术有限公司 filed Critical 成都科林分析技术有限公司
Priority to JP2017526577A priority Critical patent/JP6346379B2/ja
Priority to US15/538,163 priority patent/US10281372B2/en
Publication of WO2017113625A1 publication Critical patent/WO2017113625A1/zh

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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
    • G01N1/2226—Sampling from a closed space, e.g. food package, head space
    • 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
    • G01N1/24—Suction devices
    • 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
    • G01N1/2226—Sampling from a closed space, e.g. food package, head space
    • G01N2001/2229—Headspace sampling, i.e. vapour over liquid

Definitions

  • the invention belongs to the technical field of analysis, and particularly relates to a multi-channel headspace extraction needle.
  • the headspace injection is to seal the sample in the headspace bottle, and the object to be extracted is volatilized into the upper space of the headspace bottle by heating. Under certain conditions, the concentration of the volatile matter in the upper space of the bottle and the concentration in the sample are established. Balance, determine the concentration of the sample by extracting the upper gas from the bottle for analytical testing. The gas in the upper space of the headspace bottle should be extracted and transferred to the gas chromatograph for analysis.
  • the extraction needle is one of the key components of the whole extraction mechanism. The structure of the needle can determine the transfer mode of the entire extraction mechanism.
  • the needle is inserted into the headspace bottle to pressurize the sample (adding the carrier gas) and the sample is taken out through a single-channel needle. As the sample gas is drawn out, the bottle is filled. The pressure will be reduced, and the transfer of the headspace gas will also need to be over-extended by a large number of external components. These components will not only adsorb part of the sample, but also the sample will spread to all possible space, resulting in loss and residue of the sample. The minimum detection limit is too High, poor linear relationship, etc.
  • the dual flow needle used in the AutoHS ⁇ automatic headspace sampler overcomes the shortcomings of the pressure drop in the headspace bottle during the injection process, and also creates conditions for direct sample extraction, in order to further reduce the area of the sample contact parts as much as possible.
  • the transfer of the sample is always confined in the ideal straight-through pipe, but when the pressure inside the bottle is equal to the carrier gas pressure after pressurizing the headspace bottle, the volatile material may diffuse into the carrier gas pipe through the pipe as in the conventional headspace. road.
  • Traditional commercial headspace When the needle is inserted into the headspace bottle, the headspace bottle is pressurized. When the pressure reaches the pressure inside the bottle equal to the carrier gas pressure, the volatile substances will diffuse into the carrier gas pipeline in the opposite direction, causing certain adsorption and residue.
  • the object of the present invention is to overcome the deficiencies of the prior art, to provide a greatly reduced residue of the sample in the headspace extraction system, to ensure the integrity of the sample extraction and the pre-stage transmission, to minimize the loss of the sample, and to maintain the pressure stability.
  • Multi-channel headspace extraction needle Multi-channel headspace extraction needle.
  • the multi-channel headspace extraction needle of the invention comprises an inner needle tube, a sealing joint head, a needle rod and an outer needle tube respectively mounted on the top and bottom of the sealing joint head, and the first joint tube respectively communicating with the outer needle tube lumen on the sealing joint head
  • the second tube, the inner needle tube extends into the outer needle tube lumen and has a sealing layer between the lower end tube wall and the outer needle tube wall, and the upper end of the inner needle tube passes upward through the first tube, the second tube and the outer needle tube lumen
  • the upper portion of the sealing connector is sealed and connected to the sealing connector.
  • On the outer tube wall there are a first through hole communicating with the outer needle tube lumen at the top and the bottom of the sealing layer, and a communicating with the inner needle tube lumen. Two through holes.
  • the first pipeline and the second pipeline are on the same axis.
  • the first line, the second line, and the inner needle are in an exchangeable position, and the first line and the second line are on the sealing joint, and their intersection is at a point where the needle can work.
  • the closest distance of the tip that is, the closest distance between the thermostat area of the sample vial and the upper part of the isolation layer of the needle constant temperature after the needle is inserted into the top empty bottle; the first line, the second line and the inner needle are different from the end of the needle assembly.
  • the functional valves are connected to each other, and the direction of gas flow and the size of the gas flow can be changed by switching and switching the valves.
  • the carrier gas When the carrier gas enters the outer needle tube lumen from the first pipeline or the second pipeline to pressurize the top empty bottle, a certain flow of carrier gas always enters from the first pipeline and flows out from the second pipeline. Is controlled by the connected parts, so that the sample in the headspace bottle can be made
  • the gas does not enter the first pipeline or the second pipeline - the carrier gas input pipeline and the associated carrier gas control system, thereby avoiding the residual gas generated by the sample gas contacting the carrier gas pipeline, and extracting in the next sample.
  • the residue When the pressure is carried, the residue is brought into the next sample, which affects the accuracy of the analysis result.
  • the pressure inside the bottle is equal to the carrier gas pressure
  • the inner tube of the valve control can directly communicate with the sample transfer tube to sample.
  • the equipment delivered to the gas chromatograph or the sample that needs to receive the sample will reduce the pressure inside the bottle during the transfer, while the second or first line will also replenish the carrier gas to push the sample gas out, keeping the pressure inside the bottle stable;
  • the valve connected to the inner needle can also be directly connected to the atmosphere to achieve gas replacement. After the work is completed, the flow of the air is changed by the control of the valve, and the various pipes of the needle are purged and cleaned.
  • the multi-channel of the invention is on the needle component, not the pipeline connected thereto, which reduces the contact area between the sample and the device, and has the advantage of minimizing the residual of the sample in the headspace extraction system. It guarantees the integrity of sample extraction and pre-stage transmission, minimizes sample loss during sample extraction and transfer, and also has the advantages of gas displacement and dynamic compensation injection.
  • Figure 1 is a schematic view of the structure of the present invention.
  • Fig. 2 is an enlarged view of a portion A of Fig. 1;
  • Fig. 3 is an enlarged view of a portion B in Fig. 1.
  • Figure 4 is a left side view of Figure 1.
  • Figure 5 is a schematic view showing the pressurization of the headspace bottle of the present invention.
  • the symbol 1 represents the inner needle tube
  • the symbol 2 represents the sealing connector
  • the symbol 3 represents the needle bar
  • the symbol 4 represents the outer needle
  • the symbol 5 represents the outer needle lumen
  • the symbol 6 The first line of the table
  • the symbol 7 represents the second line
  • the symbol 8 represents the sealing layer
  • the symbol 9 represents the first through hole
  • the symbol 10 represents the second through hole
  • the symbol 11 represents the headspace bottle.
  • the multi-channel headspace extraction needle of the embodiment comprises an inner needle tube 1, a sealing joint 2, and a needle rod 3 and an outer needle tube 4 respectively mounted on the top and bottom of the sealing joint.
  • the sealing connector has a first conduit 6 and a second conduit 7 on the same horizontal plane and on the same axis respectively communicating with the outer needle lumen 5.
  • the inner needle tube extends into the outer needle tube lumen and the sealing layer 8 is arranged between the lower end tube wall and the outer needle tube wall, and the upper end of the inner needle tube passes the first tube, the second tube and the outer needle tube lumen intersection to reach the seal.
  • the upper portion of the connector is sealingly connected to the sealing connector.
  • On the outer tube wall there are a first through hole 9 communicating with the outer needle tube lumen at the top and the bottom of the sealing layer, and a second through hole 10 communicating with the inner needle tube lumen.
  • Figure 5 is a schematic view showing the pressurization of the headspace bottle 11 of the present invention.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

一种多通道顶空提取针，包括内针管（1）、密封连接头（2）、分别装在密封连接头（2）顶部和底部上的针杆（3）、外针管（4），密封连接头（2）上有分别与外针管（4）管腔连通的第一管路（6）、第二管路（7），内针管（1）伸入外针管（4）管腔内的下端管壁与外针管管壁间装有密封层（8），内针管（1）上端向上通过第一管路（6）、第二管路（7）和外针管（4）管腔交汇处后到达密封连接头（2）的上部与密封连接头（2）密封连接，在外针管（4）管壁上在位于密封层（8）的顶部、底部分别有与外针管（4）管腔相通的第一通孔（8）、与内针管（1）管腔相通的第二通孔（10）。该提取针大大减少样品在顶空提取系统中的残留，保证样品提取和前级传输的完整性，将样品的损失降到最小，保持压力稳定。

Description

多通道顶空提取针 技术领域
本发明属于分析技术领域，特别涉及的是一种多通道顶空提取针。
背景技术
顶空进样是将样品密闭在顶空瓶内，通过加热使待提取物挥发进入顶空瓶的上部空间，在一定条件下挥发物在瓶内上部空间的浓度与样品中的浓度建立一种平衡，通过提取瓶内上部气体进行分析检测来确定样品的浓度。要把顶空瓶内上部空间的气体按分析要求提取转移到气相色谱仪进行分析，提取针是整个提取机构的关键部件之一，针的结构可以决定整个提取机构的转移方式。
现代商业顶空的提取机构绝大部分是单通道的，针插入顶空瓶对样品加压(加入载气)和引出样品都是通过单通道的针完成，随着样品气体的引出，瓶内压力会降低，顶空气体的转移也需要借助大量的外部部件过度，这些部件不仅仅会吸附部分样品，而且样品会扩散到所有可能到达的空间，造成样品的损失和残留，最低检出限太高、线性关系差等。AutoHS仩自动顶空进样器采用的双流路针，克服了进样过程中顶空瓶内压力降低的缺点，也为样品直接引出创造了条件，为了进一步尽可能减少样品接触部件的面积，使样品的传递始终被约束在理想的直通管道内，但当给顶空瓶加压后瓶内压力等于载气压力时，挥发性物质如同传统顶空一样可能通过该管路反向扩散进入载气管路。传统的商业顶空 在针插入顶空瓶内对顶空瓶加压，当加压达到瓶内压力等于载气压力时，挥发性物质会反向扩散进入载气管路，造成一定的吸附和残留。
发明内容
本发明的目的是为了克服现有技术的不足，提供一种大大减少样品在顶空提取系统中的残留，保证样品提取和前级传输的完整性，将样品的损失降到最小，保持压力稳定的多通道顶空提取针。
本发明的目的是这样来实现的：
本发明多通道顶空提取针，包括内针管、密封连接头、分别装在密封连接头顶部和底部上的针杆、外针管，密封连接头上有分别与外针管管腔连通的第一管路、第二管路，内针管伸入外针管管腔内的下端管壁与外针管管壁间有密封层，内针管上端向上通过第一管路、第二管路和外针管管腔交汇处后到达密封连接头的上部与密封连接头密封连接，在外针管管壁上在位于密封层的顶部、底部分别有与外针管管腔相通的第一通孔、与内针管管腔相通的第二通孔。
上述的第一管路、第二管路在同一轴线。
使用本发明时，第一管路、第二管路、内针管是可以交换位置的，并且第一管路和第二管路是在密封连接头上，它们的交汇处处于针可以工作的离针尖最近的距离，即当针插入顶空瓶后在样品瓶恒温区和针恒温区隔离层上部最近的距离；第一管路、第二管路和内针管在离开针组件的一端都与不同功能的阀相连接，通过阀的开关和切换可以改变气体流动方向和气流大小。当载气从第一管路或第二管路进入外针管管腔对顶空瓶加压过程中，始终有一定流量的载气从第一管路进入、第二管路的流出，这个流量是由连接的部件控制的，这样就能使顶空瓶内的样品 气体不至于进入第一管路或第二管路—载气输入管路及与之相关联的载气控制系统，也就避免了产生样品气体接触到载气管路产生残留、在下一个样品提取加压时把残留带入下一个样品，影响分析结果准确性；当载气对顶空瓶加压完成后，瓶内压力等于载气压力，又阀控制内针管可以直接与样品传输管连通把样品输送到气相色谱仪或需要接收样品的设备，传输过程中瓶内压力会降低，而第二管路或第一管路也同时补充载气推动样品气体流出，保持瓶内压力稳定；当控制与内针管连接的阀也可以直接通大气，实现气体置换。工作完毕，通过阀的控制，改变气流流向，对针的各个管路吹扫、清洗。
本发明多通道是在针部件上，而不是与之连接的管路上，减少了样品与设备的接触面积，所带来的好处是最大限度地减少了样品可能在顶空提取系统中的残留，保证了样品提取和前级传输的完整性，将样品在样品的提取和传输过程中的损失降到最低，同时也具备气体置换和动态补偿进样的优点。
附图说明
图1为本发明结构示意图。
图2为图1的A部放大图。
图3为图1中B部放大图。
图4为图1的左视图。
图5为本发明对顶空瓶加压示意图。
在图1到图5中，符号1代表内针管，符号2代表密封连接头，符号3代表针杆，符号4代表外针，符号5代表外针管管腔，符号6代 表第一管路，符号7代表第二管路，符号8代表密封层，符号9代表第一通孔，符号10代表第二通孔，符号11代表顶空瓶。
以下通过具体实施例来进一步说明本发明，但实施例仅用于说明，并不能限制本发明的范围，所有对本发明的改进均在本发明的范围内，受权利要求的限制。
具体实施方式
参见图1～图4，本实施例多通道顶空提取针，包括内针管1、密封连接头2、分别装在密封连接头顶部和底部上的针杆3、外针管4。密封连接头上有位于同一水平面且同一轴线上的分别与外针管管腔5连通的第一管路6、第二管路7。内针管伸入外针管管腔内的下端管壁与外针管管壁间装有密封层8，而内针管上端向上通过第一管路、第二管路和外针管管腔交汇处后到达密封连接头的上部与密封连接头密封连接。在外针管管壁上在位于密封层的顶部、底部分别有与外针管管腔相通的第一通孔9、与内针管管腔相通的第二通孔10。
图5为本发明对顶空瓶11加压示意图。

Claims (2)

  1. 多通道顶空提取针，其特征在于包括内针管、密封连接头、分别装在密封连接头顶部和底部上的针杆、外针管，密封连接头上有分别与外针管管腔连通的第一管路、第二管路，内针管伸入外针管管腔内的下端管壁与外针管管壁间装有密封层，内针管上端通过第一管路、第二管路和外针管管腔交汇处后到达密封连接头的上部与密封连接头密封连接，在外针管管壁上在位于密封层的顶部、底部分别有与外针管管腔相通的第一通孔、与内针管管腔相通的第二通孔。
  2. 如权利要求1所述的多通道顶空提取针，其特征在于第一管路、第二管路轴线在同一轴线上。
PCT/CN2016/085695 2015-12-28 2016-06-14 多通道顶空提取针 WO2017113625A1 (zh)

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JP2017526577A JP6346379B2 (ja) 2015-12-28 2016-06-14 複数岐路を有するヘッドスペース抽出針
US15/538,163 US10281372B2 (en) 2015-12-28 2016-06-14 Multi-channel headspace extraction needle

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CN201521097015.0U CN205228898U (zh) 2015-12-28 2015-12-28 多通道顶空提取针
CN201521097015.0 2015-12-28

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CN105606409B (zh) * 2015-12-28 2018-06-05 成都科林分析技术有限公司 多通道顶空提取针
CN107702949A (zh) * 2017-08-15 2018-02-16 杭州臻盛科技有限公司 顶空取样针以及取样方法

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