阅读说明：本技术 一种气体真空进样仪及应用 (Gas vacuum sample introduction instrument and application ) 是由 吴树荣 刘蓁 于 2020-06-05 设计创作，主要内容包括：本发明公开了一种气体真空进样仪及应用,本气体真空进样仪结构简单可靠,真空进样仪内部管路死体积低(500微升至10毫升),本气体真空进样仪可以完全独立运行,可以与任何品牌气相色谱仪或其他气体分析仪器相连,不对原有的气体分析仪器进行任何硬件及软件改动即可完成气体的准确进样分析。(The invention discloses a gas vacuum sample injection instrument and application, the gas vacuum sample injection instrument has simple and reliable structure, the dead volume of an internal pipeline of the vacuum sample injection instrument is low (500 microliter to 10 milliliters), the gas vacuum sample injection instrument can completely and independently operate and can be connected with any brand gas chromatograph or other gas analysis instruments, and the accurate sample injection analysis of gas can be completed without changing any hardware and software of the original gas analysis instrument.)

1. A gas vacuum sample introduction instrument and application are characterized in that: the method comprises the following steps: the device comprises a gas switch valve (2), an eight-way flow path control valve (3), a six-way sampling valve (4), a quantitative ring (5), a carrier gas flow controller (6), a precise pressure sensor (7), a precise vacuum gauge (8), a vacuum pump (11), a temperature-controllable constant temperature valve box (19) in the vacuum sampling instrument and a vacuum pump outlet waste gas absorption device (18).

2. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that:

the sample steel cylinder (1) is connected with the gas switch valve (2).

3. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that:

the connection mode of the eight-channel control valve (3) is as follows: the first opening is connected with a precise pressure sensor (7), the second opening is connected with a sixth opening of a sample injection valve (4), the fifth opening is connected with a fifth opening of the sixth opening of the sample injection valve (4), the sixth opening is connected with a gas switch valve (2), and the seventh opening is connected with a large-caliber stainless steel pipeline (9).

4. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that:

the connection mode of the six-way sampling valve (4) is as follows: the fifth port is connected with the fifth port of the eight-through-flow-path control valve (3), and the sixth port is connected with the sixth port of the eight-through-flow-path control valve (3).

5. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that:

a large-caliber stainless steel pipeline (9) is simultaneously connected with a precision vacuum gauge (8) and a third seventh opening of an eight-way control valve (3); furthermore, the large-caliber stainless steel pipeline (9) is externally connected with a vacuum pump corrugated pipe (10); the vacuum pump corrugated pipe (10) is connected with a vacuum pump (11); the outlet of the vacuum pump (11) is connected with an exhaust gas absorption device (18).

6. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that:

the sample gas transmission line (12) is inserted into a gas chromatograph injection port (13), and two ends of a gas chromatograph chromatographic column (14) are respectively connected with the gas chromatograph injection port (13) and a gas chromatograph detector (15).

7. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that:

the device comprises a gas switch valve (2), an eight-way flow path control valve (3), a six-way sampling valve (4), a quantitative ring (5) and a precise pressure sensor (7), which are all arranged in a temperature-controllable constant temperature valve box (19) in a vacuum sampling instrument.

8. The gas vacuum sample introduction instrument and the application thereof according to claim 2 are characterized in that:

after the sample steel cylinder (1) is connected to the gas switch valve (2), the steel cylinder switch is in a closed state, the gas switch valve (2) is opened, the vacuum pump (11) is opened, the whole pipeline is vacuumized by the vacuum pump (11), the vacuum degree is read by the precision vacuum gauge (8), when the vacuum degree meets the requirement, the eight-way control valve (3) is rotated, then the sample steel cylinder (1) is opened, the quantitative ring (5) and the precision pressure sensor (7) are filled with the sample gas, the reading (7) of the precision pressure sensor is read, after the reading of the precision pressure sensor (7) is stable, the gas switch valve (2) is closed, the eight-way control valve (3) is rotated again, the whole pipeline is vacuumized again by the vacuum pump (11), the sample gas is repeatedly filled for multiple times, and; cleaning the whole pipeline by using sample gas; then filling the quantitative ring (5) and the precise pressure sensor (7) with the sample gas again, and reading and recording the reading of the precise pressure sensor (7); the volume of the gas is greatly influenced by the temperature, so that a gas switch valve (2), an eight-way flow path control valve (3), a six-way sampling valve (4), a quantitative ring (5) and a precise pressure sensor (7) are all arranged in a temperature-controllable constant-temperature valve box in a vacuum sampling instrument; the actual sample injection amount can be calculated by reading the temperature value of a temperature-controllable constant temperature valve box (19) in the vacuum sample injection instrument and the reading value of a precision pressure sensor (7); then the six-way sampling valve (4) is rotated, the carrier gas provided by the carrier gas flow controller (6) outputs the sample gas in the quantitative ring (5) to a sample inlet (13) of a gas chromatograph through a sample transmission line (12), and the sample gas enters a chromatographic column (14) of the gas chromatograph through the sample inlet (13) of the gas chromatograph for separation and then enters a detector (15) of the gas chromatograph for detection.

9. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that: the gas vacuum sample injection instrument can be integrally installed on the gas chromatograph.

10. The gas vacuum sample introduction instrument and the application thereof according to claim 1 are characterized in that: the use of a gas vacuum sampler for the determination of gas samples, including, without limitation: a common, non-toxic, hazardous gas sample; toxic, harmful, corrosive gas samples.

Technical Field

The invention relates to gas sample injection analysis, in particular to a gas vacuum sample injection instrument and application thereof.

Background

Analysis of gas samples is widely used in various fields: chemical plants, petroleum and petrochemical industries, geological exploration, environmental monitoring, scientific research institutions and other industries. The currently common gas sampling mode is generally as follows: sampling by an air bag, sampling by a steel cylinder and sampling by a gas collecting tank. With the progress of science and technology, the traditional gas sampling mode increasingly faces the following problems:

1, common non-toxic and harmful gas samples can be sampled through the air bag, then the air bag is connected with a gas injection port of a gas chromatograph, a gas chromatograph-mass spectrometer or other gas analyzers, and the gas samples are extruded to the analyzers for analysis in a mode of extruding the air bag. However, the air bag sample injection mode has a problem which cannot be solved: samples with extremely small sample size, such as only a few milliliters of sample, cannot fill the air pocket, and are difficult to inject by extrusion.

2, to the toxicity that meets in chemical plant or environmental monitoring, harmful, have corrosive gas sample, adopt the sampling steel bottle sampling usually, the sampling steel bottle has the firm, and good sealing performance can avoid revealing the risk, but still faces a problem and can't solve:

the sampling steel cylinder can not adopt an extrusion mode for sample injection like an air bag, so the gas pressure in the sampling steel cylinder is required to be larger than the atmospheric pressure after the sampling is finished, and the gas pressure in the sampling steel cylinder is required to be more than two atmospheric pressures in general in order to meet the requirement of at least 2-3 times of repeated measurement of one sample. Thus, the pressure of the sample gas source is required to be more than two atmospheres, but the gas source for environmental pollution and the gas pressure of the corrosive gas sample are toxic and harmful to a plurality of chemical plants, and are both normal pressure, namely one atmosphere, so that the gas sample in the steel cylinder is difficult to be injected into a gas analyzer.

For some scientific research institutions, experimental gas samples generated by the experimental device are very rare, usually only a few milliliters, and some gas samples have high value and cannot be sampled in gas steel cylinders, gas bags and other modes. Many researchers in scientific research institutions are looking for a gas sample injection instrument which can be directly connected with an experimental device, has an extremely low dead volume, can accurately read sample injection pressure and calculate accurate sample injection amount.

The invention aims to overcome the defects of the prior art, provides a gas vacuum sample injection instrument, can meet the relevant national standards, can utilize the existing gas chromatograph of any brand or other gas analyzers, and can complete sample injection analysis on various toxic, harmful, corrosive, rare and precious gas samples with the sample pressure lower than the atmospheric pressure.

Technical scheme

The invention relates to a gas vacuum sample injection instrument and application thereof: the method comprises the following steps: the device comprises a gas switch valve (2), an eight-way flow path control valve (3), a six-way sampling valve (4), a quantitative ring (5), a carrier gas flow controller (6), a precise pressure sensor (7), a precise vacuum gauge (8), a vacuum pump (11), a temperature-controllable constant temperature valve box (19) in the vacuum sampling instrument and a vacuum pump outlet waste gas absorption device (18).

The invention relates to a gas vacuum sample injection instrument and application thereof:

the sample steel cylinder (1) is connected with the gas switch valve (2).

The invention relates to a gas vacuum sample injection instrument and application thereof:

the connection mode of the eight-channel control valve (3) is as follows: the first opening is connected with a precise pressure sensor (7), the second opening is connected with a sixth opening of a sample injection valve (4), the fifth opening is connected with a fifth opening of the sixth opening of the sample injection valve (4), the sixth opening is connected with a gas switch valve (2), and the seventh opening is connected with a large-caliber stainless steel pipeline (9).

The invention relates to a gas vacuum sample injection instrument and application thereof:

the connection mode of the six-way sampling valve (4) is as follows: the fifth port is connected with the fifth port of the eight-through-flow-path control valve (3), and the sixth port is connected with the sixth port of the eight-through-flow-path control valve (3).

The invention relates to a gas vacuum sample injection instrument and application thereof:

a large-caliber stainless steel pipeline (9) is simultaneously connected with a precision vacuum gauge (8) and a third seventh opening of an eight-way control valve (3); furthermore, the large-caliber stainless steel pipeline (9) is externally connected with a vacuum pump corrugated pipe (10); the vacuum pump corrugated pipe (10) is connected with a vacuum pump (11); the outlet of the vacuum pump (11) is connected with an exhaust gas absorption device (18).

The invention relates to a gas vacuum sample injection instrument and application thereof:

the sample gas transmission line (12) is inserted into a gas chromatograph injection port (13), and two ends of a gas chromatograph chromatographic column (14) are respectively connected with the gas chromatograph injection port (13) and a gas chromatograph detector (15).

The invention relates to a gas vacuum sample injection instrument and application thereof:

the device comprises a gas switch valve (2), an eight-way flow path control valve (3), a six-way sampling valve (4), a quantitative ring (5) and a precise pressure sensor (7), which are all arranged in a temperature-controllable constant temperature valve box (19) in a vacuum sampling instrument.

The invention relates to a gas vacuum sample injection instrument and application thereof:

after the sample steel cylinder (1) is connected to the gas switch valve (2), the steel cylinder switch is in a closed state, the gas switch valve (2) is opened, the vacuum pump (11) is opened, the whole pipeline is vacuumized by the vacuum pump (11), the vacuum degree is read by the precision vacuum gauge (8), when the vacuum degree meets the requirement, the eight-way control valve (3) is rotated, then the sample steel cylinder (1) is opened, the quantitative ring (5) and the precision pressure sensor (7) are filled with the sample gas, the reading of the precision pressure sensor (7) is read, after the reading of the precision pressure sensor (7) is stable, the gas switch valve (2) is closed, the eight-way control valve (3) is rotated again, the whole pipeline is vacuumized again by the vacuum pump (11), the sample gas is repeatedly filled for multiple times, and then; cleaning the whole pipeline by using sample gas; then filling the quantitative ring (5) and the precise pressure sensor (7) with the sample gas again, and reading and recording the reading of the precise pressure sensor (7); the volume of the gas is greatly influenced by the temperature, so that a gas switch valve (2), an eight-way flow path control valve (3), a six-way sampling valve (4), a quantitative ring (5) and a precise pressure sensor (7) are all arranged in a temperature-controllable constant-temperature valve box (19) in a vacuum sampling instrument; the actual sample injection amount can be calculated by reading the temperature value of the temperature-controllable constant temperature valve box (19) of the vacuum sample injection instrument and the reading value of the precision pressure sensor (7); then the six-way sampling valve (4) is rotated, the carrier gas provided by the carrier gas flow controller (6) outputs the sample gas in the quantitative ring (5) to a sample inlet (13) of a gas chromatograph through a sample transmission line (12), and the sample gas enters a chromatographic column (14) of the gas chromatograph through the sample inlet (13) of the gas chromatograph for separation and then enters a detector (15) of the gas chromatograph for detection.

The invention relates to a gas vacuum sample injection instrument: the gas vacuum sample injection instrument can be integrally installed on the gas chromatograph.

The invention relates to a gas vacuum sample injection instrument and application thereof, which are divided into two modes: (1) with gas injection valve mode: aiming at a gas chromatograph or other gas analysis instruments which are not provided with a gas injection valve; (2) no gas injection valve mode: for gas chromatographs or other gas analysis instruments that have been equipped with gas injection valves.

A gas vacuum sample introduction instrument relates to a gas sample introduction valve mode: aiming at a gas chromatograph or other gas analysis instruments which are not provided with a gas injection valve;

the sample valve with gas injection mode comprises two modules: a vacuum system module with a sample injection valve and a control circuit module.

The vacuum system module with the sample injection valve comprises: carrier gas flow controller, gas sample injection valve, gas flow path control valve, precision pressure sensor, precision vacuum gauge, vacuum pump, connecting pipeline and valve. The number of the gas flow path control valves is p (p is more than or equal to 1 and less than or equal to 15), and one end of the outlet of the gas injection valve outputs a sample to any brand gas chromatograph or other gas analysis instruments through a zero dead volume connector.

The control circuit module includes: control circuit board (optionally join in marriage on the circuit board and install USB, LAN, WIFI, bluetooth module), power strip, touch liquid crystal display.

Gas vacuum appearance of advancing relates to and does not take gas injection valve mode: for gas chromatographs or other gas analysis instruments that have been equipped with gas injection valves.

The no gas injection valve mode includes two modules: a vacuum system module and a control circuit module. The vacuum system module includes: the device comprises a gas flow path control valve, a precise pressure sensor, a precise vacuum gauge, a vacuum pump, a connecting pipeline and a valve. The number of the gas flow path control valves is p (p is more than or equal to 1 and less than or equal to 15), and one end of the outlet of the gas injection valve is connected with the gas injection valve of any brand gas chromatograph or other gas analyzers through a pipeline. The control circuit module includes: control circuit board (optionally join in marriage on the circuit board and install USB, LAN, WIFI, bluetooth module), power strip, touch liquid crystal display.

The gas vacuum sample introduction instrument has simple and reliable structure, the dead volume of the internal pipeline of the vacuum sample introduction instrument is low (500 microliter to 10 milliliters), the gas vacuum sample introduction instrument can completely and independently operate and can be connected with any brand gas chromatograph or other gas analyzers, and the gas sample introduction can be completed without changing any hardware and software of the original analysis instrument. The user can select the valve of different materials, the pipeline connects according to the needs of waiting to analyze the sample, also can revise gas flow path design according to the demand to realize the analysis demand of different application environment.

Further, the analysis module uses m n-way sample and flow control valves. (1 is more than or equal to m and less than or equal to 14, and 2 is more than or equal to n and less than or equal to 14), the number and the types of different valves can be selected according to the types of the samples.

Furthermore, the vacuum sample injection system is connected with any brand gas chromatograph or other gas analysis instruments through pipelines.

The application of a gas vacuum sample injection instrument comprises the following steps: the use of a gas vacuum sampler for the determination of gas samples, including, without limitation: a common, non-toxic, hazardous gas sample; toxic, harmful, corrosive gas samples.

The invention has the following beneficial effects:

the gas vacuum sample introduction instrument can completely and independently operate, can be connected with any brand gas chromatograph or other gas analysis instruments, can select different vacuum sample introduction system modes according to whether the existing gas chromatograph or other gas analysis instruments are provided with gas sample introduction valves or not, does not need to modify the existing analyzer or add a special sample introduction system, and saves the cost.

The gas vacuum sample introduction instrument can be customized according to customer requirements, and different materials, different calibers and different connection modes are selected. The method can provide solutions for industries such as environmental monitoring, chemical plants, industrial production, hydrogen energy sources, scientific research institutions and the like.

The type and number of the sample introduction/flow path control valves are selected in various ways, so that not only can the vacuum sample introduction of the sample be realized, but also a pretreatment chromatographic column can be added according to the requirement, the functions of sample pretreatment, back flushing, cutting and the like can be realized, and the sample introduction/flow path control valves are applied to the sample introduction analysis of various special gas samples.

The dead volume of the internal pipeline of the gas vacuum sample introduction instrument is low (500 microliters to 10 milliliters), and the gas vacuum sample introduction instrument is suitable for sample introduction analysis of a small amount of precious gas samples, is simple in structure, adopts multi-way valve design, and achieves a better vacuum effect through multi-point vacuumizing.

The gas vacuum sample introduction instrument comprises the following relevant standards which relate to but are not limited to:

1. GB/T6681 and 2003 gas chemical product sampling general rule

2. Method for sampling particulate matters and gaseous pollutants in exhaust gas of GB/T16157 and 1996 fixed pollution source

3. GBZ 159 specification for sampling harmful substance monitoring in air of 2004 workplace

4. GB 13733 and 1992 air sampling regulations for toxic workplaces

The gas vacuum sample introduction instrument can be suitable for any brand gas chromatograph or other gas analyzers. The customer only needs a gas vacuum sample introduction instrument, and can be connected with any brand gas chromatograph or other gas analyzers for use, and the accurate sample introduction analysis of various poisonous, harmful, corrosive and rare gas samples is completed.

Drawings

FIG. 1: a vacuum sample injection instrument (with a gas sample injection valve mode) and a gas chromatograph (without a gas sample injection valve) are connected schematically;

FIG. 2: the connection schematic diagram of a vacuum sample injection instrument (without a gas injection valve mode) and a gas chromatograph (provided with a gas injection valve already);

FIG. 3: schematic diagram of vacuum sample injection instrument control module (with gas sample injection valve mode and without gas sample injection valve mode):

FIG. 4: schematic diagram of a vacuum sample introduction instrument for controlling a touch liquid crystal screen:

FIG. 5: schematic diagram of replacing eight-way valve with two four-way valves

FIG. 6: schematic diagram of replacing eight-way valve with two four-way valves

Detailed explanation of the attached FIGS. 1-6

FIG. 1 is a detailed explanation of a vacuum sample injection instrument (with gas injection valve mode) and a gas chromatograph (without gas injection valve) connection diagram

1: sample steel cylinder

2: gas switch valve

3: eight-way flow control valve

4: six-way sample injection valve

5: quantitative ring

6: carrier gas flow controller

7: precision pressure sensor

8: precision vacuum gauge

9: heavy gauge stainless steel tubing (1/8 inch, 1/4 inch or larger gauge)

10: vacuum pump bellows

11: vacuum pump

12: sample gas transmission line

13: sample inlet of gas chromatograph

14: gas chromatograph chromatographic column

15: gas chromatograph detector

16: vacuum sample introduction instrument

17: gas chromatograph

18: exhaust gas absorption device

19: temperature-controllable constant temperature valve box in vacuum sample injection instrument

The connection mode of the eight-channel control valve (3) is as follows: the first opening is connected with a precise pressure sensor (7), the second opening is connected with a sixth opening of a sample injection valve (4), the fifth opening is connected with a fifth opening of the sixth opening of the sample injection valve (4), the sixth opening is connected with a gas switch valve (2), and the seventh opening is connected with a large-caliber stainless steel pipeline (9).

The connection mode of the six-way sampling valve (4) is as follows: the fifth port is connected with the fifth port of the eight-through-flow-path control valve (3), and the sixth port is connected with the sixth port of the eight-through-flow-path control valve (3).

FIG. 2 (detailed explanation of the vacuum injector (without gas injection valve mode) and gas chromatograph (already equipped with gas injection valve) connections);

1: sample steel cylinder

2: gas switch valve

3: eight-way flow control valve

4: six-way sample injection valve in gas chromatograph

5: quantitative ring in gas chromatograph

6: carrier gas flow controller in gas chromatograph

7: precision pressure sensor

8: precision vacuum gauge

9: heavy gauge stainless steel tubing (1/8 inch, 1/4 inch or larger gauge)

10: vacuum pump bellows

11: vacuum pump

14: gas chromatograph chromatographic column

15: gas chromatograph detector

16: vacuum sample introduction instrument

17: gas chromatograph

18: exhaust gas absorption device

19: temperature-controllable constant temperature valve box in vacuum sample injection instrument

20: temperature-controllable thermostatic valve box in gas chromatograph

FIG. 3 is a schematic view showing the control module of the vacuum sample injection instrument (with and without gas injection valve mode)

21: power supply module

22: controller of precision vacuum gauge

23: precise pressure sensor controller

24: temperature controller

25: control main circuit board

26: touch liquid crystal screen

27: LAN module

28: USB module

29: WIFI Module

30: bluetooth module

Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Detailed Description