Automatic headspace sample injector for parallel sample injection

文档序号:733860 发布日期:2021-04-20 浏览:3次 中文

阅读说明:本技术 一种平行进样的自动顶空进样器 (Automatic headspace sample injector for parallel sample injection ) 是由 吴火平 李其淦 于 2021-01-11 设计创作,主要内容包括:本发明涉及气相色谱分析领域,尤指一种平行进样的自动顶空进样器,包含:十通阀、第一定量环、第二定量环、第一色谱柱、第二色谱柱、第一FID检测器、第二FID检测器、第一GC进样口以及第二GC进样口,所述十通阀与所述第一定量环、第二定量环、第一FID检测器以及第二FID检测器连通;所述十通阀的十个阀口按顺序依次为1号口、2号口、3号口、4号口、5号口、6号口、7号口、8号口、9号口和10号口,所述4号口连通有第二色谱载气装置,所述7号口连通有样品出口,所述8号口连通有样品入口,所述10号口连通有第一色谱载气装置。本发明可以将同一份气体样品平行的、同时的在两个不同的分析条件下进行测试,能够有效排除假阳性干扰。(The invention relates to the field of gas chromatography analysis, in particular to an automatic headspace sample injector for parallel sample injection, which comprises: the system comprises a ten-way valve, a first quantitative ring, a second quantitative ring, a first chromatographic column, a second chromatographic column, a first FID detector, a second FID detector, a first GC sample inlet and a second GC sample inlet, wherein the ten-way valve is communicated with the first quantitative ring, the second quantitative ring, the first FID detector and the second FID detector; the ten valve ports of the ten-way valve are sequentially a port 1, a port 2, a port 3, a port 4, a port 5, a port 6, a port 7, a port 8, a port 9 and a port 10, wherein the port 4 is communicated with a second chromatographic carrier gas device, the port 7 is communicated with a sample outlet, the port 8 is communicated with a sample inlet, and the port 10 is communicated with a first chromatographic carrier gas device. The invention can test the same gas sample in parallel and simultaneously under two different analysis conditions, and can effectively eliminate false positive interference.)

1. The utility model provides an automatic headspace sample injector of parallel injection which characterized in that contains: ten valve ports of the ten-way valve are sequentially a port 1, a port 2, a port 3, a port 4, a port 5, a port 6, a port 7, a port 8, a port 9 and a port 10,

the No. 1 port is communicated with the first FID detector through the first GC sample inlet and the first chromatographic column in sequence, the No. 4 port is communicated with the second chromatographic carrier gas device, the No. 5 port is communicated with the second FID detector through the second GC sample inlet and the second chromatographic column in sequence, the No. 7 port is communicated with the sample outlet, the No. 8 port is communicated with the sample inlet, and the No. 10 port is communicated with the first chromatographic carrier gas device;

the two ends of the first quantitative ring are respectively communicated with the No. 2 port and the No. 9 port, and the two ends of the second quantitative ring are respectively communicated with the No. 3 port and the No. 6 port.

2. The parallel sample injection autosampler according to claim 1, wherein said ten-way valve has two states of sampling and sample injection, specifically:

sampling state: the No. 8 port is communicated with the No. 9 port, the No. 10 port is communicated with the No. 1 port, the No. 2 port is communicated with the No. 3 port, the No. 4 port is communicated with the No. 5 port, and the No. 6 port is communicated with the No. 7 port;

sample introduction state: the No. 1 port is communicated with the No. 2 port, the No. 3 port is communicated with the No. 4 port, the No. 5 port is communicated with the No. 6 port, the No. 7 port is communicated with the No. 8 port, and the No. 9 port is communicated with the No. 10 port.

3. The parallel-fed auto-headspace sampler according to claim 2, wherein the parallel-fed auto-headspace sampler further comprises a first six-way valve and a second six-way valve,

and the first six-way valve and the second six-way valve are communicated with each other and are used for replacing the ten-way valve.

4. The parallel-sample auto-headspace sampler according to claim 3, wherein the six valve ports of the first six-way valve are port 11, port 12, port 13, port 14, port 15 and port 16 in this order, and the six valve ports of the second six-way valve are port 21, port 22, port 23, port 24, port 25 and port 26 in this order,

the No. 12 port is communicated with a first chromatographic carrier gas device, the No. 13 port is communicated with a first FID detector through the first GC sample inlet and the first chromatographic column in sequence, and the No. 16 port is communicated with the sample inlet;

the No. 22 port is communicated with a second chromatographic carrier gas device, the No. 23 port is communicated with a second FID detector through the second GC sample inlet and the second chromatographic column in sequence, and the No. 25 port is communicated with the sample outlet;

two ends of the first quantitative ring are respectively communicated with the No. 11 port and the No. 14 port, two ends of the second quantitative ring are respectively communicated with the No. 26 port and the No. 24 port, and the No. 15 port is communicated with the No. 21 port.

Technical Field

The invention relates to the field of gas chromatography analysis, in particular to an automatic headspace sample injector for parallel sample injection.

Background

The headspace sampler is a sample injection device for measuring the content of these components in the sample as they are by the gas composition above the sample matrix, and is an indirect measurement method, and the basic theoretical basis is as follows: under certain conditions, there is a partitioning equilibrium between the gas phase and the condensed phase (liquid or solid). The analysis principle is as follows: placing the sample in a closed container, placing the sample at a certain temperature for a period of time to make the gas-liquid two phases reach equilibrium, and taking the gas phase part to enter GC analysis.

The main application range is as follows:

1. the analyte to be detected volatilizes below 200 ℃;

2. the sample to be analyzed is solid, paste or liquid, and can enter the GC sample inlet after sample pretreatment;

3. the operating environment makes it difficult to perform reliable sample pre-processing.

In some special application occasions, such as drunk driving, the judicial identification standard method SF/Z JD 0107001-2016 uses two different chromatographic columns to prepare two blood samples of the same person, and two headspace sampling analyses are needed to analyze the ethanol peak time in the prepared blood so as to eliminate false positive brought by other alcohols.

The headspace sampler currently on the market (for example, patent application No. CN201310240244.2, one name of which is in-situ headspace sampler) can only transfer the substance in one sample to one chromatographic column of a gas chromatograph for analysis. If parallel detection is needed under different conditions, two samples are needed, and the parallel detection can be realized only by sampling twice, so that the detection efficiency is not high, and result deviation can be brought after different samples are treated.

Therefore, the existing headspace sampler has the following technical problems:

1. two samples are needed for parallel sample injection test, and two times of sample injection are needed; the difference between the two sampled samples leads to uncertainty of the detection result;

2. in judicial identification, if a driver dies due to a traffic accident, two blood samples are difficult to extract due to the great difficulty in obtaining blood of the dead;

3. in order to realize a standard experiment, a single sample of a currently marketed headspace sample injector needs to be connected and switched with a gas chromatograph twice, so that the operation is complex, unattended operation cannot be realized, and gas leakage of the gas chromatograph is easily caused, thereby affecting the accuracy of a final detection result.

Disclosure of Invention

In order to solve the above problems, the present invention provides a parallel sample injection auto-headspace sample injector, which can perform parallel sample injection on the same sample and perform a test under two different analysis conditions, so as to effectively eliminate false positive interference and improve test efficiency and test accuracy.

In order to achieve the purpose, the invention adopts the technical scheme that:

a parallel-fed auto-headspace sampler, comprising: ten valve ports of the ten-way valve are sequentially a port 1, a port 2, a port 3, a port 4, a port 5, a port 6, a port 7, a port 8, a port 9 and a port 10,

the No. 1 port is communicated with the first FID detector through the first GC sample inlet and the first chromatographic column in sequence, the No. 4 port is communicated with the second chromatographic carrier gas device, the No. 5 port is communicated with the second FID detector through the second GC sample inlet and the second chromatographic column in sequence, the No. 7 port is communicated with the sample outlet, the No. 8 port is communicated with the sample inlet, and the No. 10 port is communicated with the first chromatographic carrier gas device;

the two ends of the first quantitative ring are respectively communicated with the No. 2 port and the No. 9 port, and the two ends of the second quantitative ring are respectively communicated with the No. 3 port and the No. 6 port.

Further, the ten-way valve has two states of sampling and sample introduction, and specifically comprises:

sampling state: the No. 8 port is communicated with the No. 9 port, the No. 10 port is communicated with the No. 1 port, the No. 2 port is communicated with the No. 3 port, the No. 4 port is communicated with the No. 5 port, and the No. 6 port is communicated with the No. 7 port;

sample introduction state: the No. 1 port is communicated with the No. 2 port, the No. 3 port is communicated with the No. 4 port, the No. 5 port is communicated with the No. 6 port, the No. 7 port is communicated with the No. 8 port, and the No. 9 port is communicated with the No. 10 port.

Further, the automatic headspace sample injector for parallel sample injection also comprises a first six-way valve and a second six-way valve,

and the first six-way valve and the second six-way valve are communicated with each other and are used for replacing the ten-way valve.

Further, the six valve ports of the first six-way valve are sequentially a port No. 11, a port No. 12, a port No. 13, a port No. 14, a port No. 15 and a port No. 16, the six valve ports of the second six-way valve are sequentially a port No. 21, a port No. 22, a port No. 23, a port No. 24, a port No. 25 and a port No. 26, wherein,

the No. 12 port is communicated with a first chromatographic carrier gas device, the No. 13 port is communicated with a first FID detector through the first GC sample inlet and the first chromatographic column in sequence, and the No. 16 port is communicated with the sample inlet;

the No. 22 port is communicated with a second chromatographic carrier gas device, the No. 23 port is communicated with a second FID detector through the second GC sample inlet and the second chromatographic column in sequence, and the No. 25 port is communicated with the sample outlet;

two ends of the first quantitative ring are respectively communicated with the No. 11 port and the No. 14 port, two ends of the second quantitative ring are respectively communicated with the No. 26 port and the No. 24 port, and the No. 15 port is communicated with the No. 21 port.

The invention has the beneficial effects that:

the ten-way valve is communicated with the first chromatographic carrier gas device, the second chromatographic carrier gas device, the first quantitative ring, the second quantitative ring, the first FID detector and the second FID detector, and a part of gas sample can be simultaneously sent to the first FID detector and the second FID detector through the ten-way valve for testing, so that the same part of gas sample can be tested under two different analysis conditions in parallel and simultaneously, false positive interference can be effectively eliminated, and the testing efficiency and the testing accuracy are improved.

The invention can use two original six-way valves for communication to replace the ten-way valve, and does not need to buy a new ten-way valve, thereby reducing the cost.

Drawings

FIG. 1 is a schematic diagram of a sampling state of the present invention.

FIG. 2 is a schematic view of the sample injection state of the present invention.

FIG. 3 is a schematic of the present invention utilizing two six-way valves instead of a ten-way valve.

The reference numbers illustrate: 101. a first quantity of rings; 102. a first chromatographic carrier gas device; 103. a first GC sample inlet; 104. a first chromatographic column; 105. a first FID detector; 106. a ten-way valve; 107. a second chromatographic carrier gas device; 108. a second FID detector; 109. a second chromatography column; 110. a second GC sample inlet; 111. a second dosing ring; 112. a sample outlet; 113. a sample inlet; 114. a first six-way valve; 115. a second six-way valve.

Detailed Description

Referring to fig. 1, the present invention relates to an auto-headspace sampler for parallel sampling, comprising: a ten-way valve 106, a first quantitative ring 101, a second quantitative ring 111, a first chromatographic column 104, a second chromatographic column 109, a first FID detector 105, a second FID detector 108, a first GC sample inlet 103 and a second GC sample inlet 110, wherein the ten valve ports of the ten-way valve 106 are sequentially a port 1, a port 2, a port 3, a port 4, a port 5, a port 6, a port 7, a port 8, a port 9 and a port 10, wherein,

the port 1 is communicated with a first FID detector 105 through a first GC sample inlet 103 and a first chromatographic column 104 in sequence, the port 4 is communicated with a second chromatographic carrier gas device 107, the port 5 is communicated with a second FID detector 108 through a second GC sample inlet 110 and a second chromatographic column 109 in sequence, the port 7 is communicated with a sample outlet 112, the port 8 is communicated with a sample inlet 113, and the port 10 is communicated with a first chromatographic carrier gas device 102;

two ends of the first quantitative ring 101 are respectively communicated with the No. 2 port and the No. 9 port, and two ends of the second quantitative ring 111 are respectively communicated with the No. 3 port and the No. 6 port.

Further, the ten-way valve 106 has two states of sampling and sample injection, specifically:

sampling state: the No. 8 port is communicated with the No. 9 port, the No. 10 port is communicated with the No. 1 port, the No. 2 port is communicated with the No. 3 port, the No. 4 port is communicated with the No. 5 port, and the No. 6 port is communicated with the No. 7 port;

sample introduction state (see fig. 2): the No. 1 port is communicated with the No. 2 port, the No. 3 port is communicated with the No. 4 port, the No. 5 port is communicated with the No. 6 port, the No. 7 port is communicated with the No. 8 port, and the No. 9 port is communicated with the No. 10 port.

The working principle is as follows:

sampling: the gas sample stored in the headspace bottle enters from the port 8 and exits from the port 9; flows through the first quantitative ring 101 and then enters the No. 2 port and exits the No. 3 port; flows through the second quantitative ring 111 and then enters the No. 6 port and exits the No. 7 port; and finally out of the sample outlet 112; this process fills both the first dosing ring 101 and the second dosing ring 111 with the same gas sample.

And (3) sample introduction: the ten-way valve 106 is switched in a rotating way, and the chromatographic carrier gas in the first chromatographic carrier gas device 102 enters from the port 10 and exits from the port 9; flows through the first quantitative ring 101 and enters the No. 2 port and exits the No. 1 port; and then sequentially passes through the first GC sample inlet 103 and the first chromatographic column 104 to reach the first FID detector 105 for analysis and detection. Meanwhile, the chromatographic carrier gas in the second chromatographic carrier gas device 107 enters from the port 4 and exits from the port 3; after flowing through the second quantitative ring 111, the mixture enters the No. 6 port and exits the No. 5 port; and then sequentially passes through the second GC sample inlet 110 and the second chromatographic column 109 to reach the second FID detector 108 for analysis and detection.

Through the sampling process and the sample introduction process, the parallel and simultaneous test of the same gas sample under two different analysis conditions is realized, and the false positive interference can be effectively eliminated.

In another embodiment of the present invention, referring to fig. 3, the parallel sample auto-headspace sampler further includes a first six-way valve 114 and a second six-way valve 115,

the first six-way valve 114 and the second six-way valve 115 communicate with each other, replacing the ten-way valve 106; it should be noted that the working principle of this embodiment is the same as that of the ten-way valve 106, and the details will not be described below;

the advantage of this embodiment is that instead of ten-way valve 106, two existing six-way valves may be used to communicate, eliminating the need to purchase a new ten-way valve 106, and reducing costs.

Further, the six valve ports of the first six-way valve 114 are, in order, port No. 11, port No. 12, port No. 13, port No. 14, port No. 15 and port No. 16, the six valve ports of the second six-way valve 115 are, in order, port No. 21, port No. 22, port No. 23, port No. 24, port No. 25 and port No. 26, wherein,

the port 12 is communicated with a first chromatographic carrier gas device 102, the port 13 is communicated with a first FID detector 105 through a first GC sample inlet 103 and a first chromatographic column 104 in sequence, and the port 16 is communicated with the sample inlet 113;

the port 22 is communicated with a second chromatographic carrier gas device 107, the port 23 is communicated with a second FID detector 108 through a second GC sample inlet 110 and a second chromatographic column 109 in sequence, and the port 25 is communicated with the sample outlet 112;

two ends of the first quantitative ring 101 are respectively communicated with the No. 11 port and the No. 14 port, two ends of the second quantitative ring 111 are respectively communicated with the No. 26 port and the No. 24 port, and the No. 15 port is communicated with the No. 21 port.

The above embodiments are merely illustrative of the preferred embodiments of the present invention, and not restrictive, and various changes and modifications to the technical solutions of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are intended to fall within the scope of the present invention defined by the appended claims.

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