CN106706816A - Vacuum sampling device for gas chromatograph - Google Patents
Vacuum sampling device for gas chromatograph Download PDFInfo
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- CN106706816A CN106706816A CN201710028251.4A CN201710028251A CN106706816A CN 106706816 A CN106706816 A CN 106706816A CN 201710028251 A CN201710028251 A CN 201710028251A CN 106706816 A CN106706816 A CN 106706816A
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- vacuum
- gas
- valve
- gas chromatograph
- sampling device
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a vacuum sampling device for a gas chromatograph. The vacuum sampling device comprises a standard gas bottle, a sample container, the gas chromatograph and a vacuum pump, wherein the standard gas bottle and the sample container are connected with a gas inlet of the gas chromatograph through gas tubes, and the vacuum pump is connected with an exhaust port of the gas chromatograph through a gas tube. A pressure sensor for measuring a pressure value in each gas tube and a vacuum gauge for measuring the vacuum degree in each gas tube are installed on each gas tube. A temperature sensor for measuring an environment temperature value is further installed. The vacuum sampling device for the gas chromatograph improves a traditional valve sampling mode of the gas chromatograph, tested sample gas pollution caused by ambient air is avoided, and the precision of quantitative analysis on components in the sample gas such as a trace amount of oxygen and nitrogen components is effectively improved. In addition, the sampling pressure can be adjusted, the phenomenon that detector response of the gas chromatograph is overloaded or too low is avoided, a response linearity range of a detector is widened, and analytical errors are decreased.
Description
Technical field
The invention belongs to gas chromatographicanalyzer technical field, and in particular to a kind of gas chromatograph is filled with vacuum sample introduction
Put.
Background technology
Gas chromatograph is widely used at aspects such as oil, chemical industry, biochemistry, medical and health, food industry, environmental protection,
Qualitative and quantitative analysis can be carried out to gas.In gas chromatographic analysis, sample introduction be quantitative analysis error main source it
One.The principle of input mode and sampling system, structure, using material, sample introduction when temperature, sample size, sample introduction speed, sample introduction use
Instrument etc. the repeatability and accuracy of the quantitative and qualitative of gas chromatographic analysis can all be had a direct impact.
Gaseous sample using commercialization valve injection system sample introduction is easy to operate, quantitative repeatability is good, but be not suitable for normal pressure,
Negative pressure sample feeding is analyzed, and is difficult to avoid that pollution of the surrounding air to gaseous sample, and analysis result is interfered, especially right
When micro amount of oxygen, nitrogen component in gaseous sample carry out quantitative analysis, oxygen, nitrogen impurity in air can severe jamming analysis knots
Really.Sample introduction circuit air is removed according to traditional Purge methods, can be taken considerable time and sample gas, and be difficult to eliminate pipeline
Air plankton.In addition, conventional valve input mode can not adjust sample introduction pressure, enriched sample component or low concentration sample group are measured
Timesharing, due to detector response overload or too low, can cause larger error to analysis result.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of gas chromatograph vacuum sampling device.
A kind of gas chromatograph vacuum sampling device of the invention, is characterized in, the device include calibrating gas gas cylinder,
Shuttle, gas chromatograph and vavuum pump, calibrating gas gas cylinder and shuttle by tracheae respectively with gas chromatograph
Air inlet is connected, and vavuum pump is connected by tracheae with the exhaust outlet of gas chromatograph；It is also equipped with temperature sensor, measuring environment
Temperature value, temperature value passes through temperature indicator meter reading；Pressure sensing is connected with by pressure sensor valve on described tracheae
Device, measures endotracheal atmospheric pressure value, and atmospheric pressure value passes through pressure display instrument meter reading；Connected by vacuum meter valve on described tracheae
There is vacuum meter, measure endotracheal vacuum, vacuum passes through vacuum display instrument reading；The exhaust of described gas chromatograph
Atmospheric valve is connected with mouthful.
Being installed in series between described calibrating gas gas cylinder and tracheae has pressure-reducing valve and gas valve.
Being installed in series between described shuttle and tracheae has filter and sample air valve.
Being installed in series between described vavuum pump and tracheae has vacuum pumping valve and bellows.
Described tracheae is stainless steel tube, and vacuum is calculated as diagram vacuum gauge, and vavuum pump is dry vacuum pump.
The air inlet pipe of described gas chromatograph and the overall leakage rate of blast pipe are less than or equal to 10-7Pa·m3/s。
Described gas chromatograph vacuum sampling device also includes a housing, described temperature sensor, pressure biography
Sensor valve and vacuum meter are installed on described enclosure interior；Described temperature display meter, pressure display instrument table, vacuum display instrument
Table, pressure sensor valve, vacuum meter, atmospheric valve, gas valve, sample air valve and vacuum pumping valve are installed on described housing front face
Plate；The power line of described temperature display meter, pressure display instrument table and vacuum display instrument is integrated into the electricity of described housing
Source switch.
Described gas valve, sample air valve, pressure sensor valve, vacuum meter valve, vacuum pumping valve and atmospheric valve are bellows valve.
Gas chromatograph vacuum sampling device of the invention improves the traditional valve injection mode of gas chromatograph, is entering
Sample introduction pipeline is vacuumized before sample, the foreign gas in removal sample introduction pipeline, it is to avoid surrounding air is to sample gas
The pollution of body, effectively increases the analysis precision of sample gas, has been improved particularly micro amount of oxygen, the essence of nitrogen measured portions analysis
Degree；Sample introduction pressure can be adjusted simultaneously, it is to avoid when measurement enriched sample component or low concentration sample component, gas chromatograph
Detector response is overloaded or responds too low, expands the detector response range of linearity, reduces analytical error, accurate with analysis
Degree is high, advantage easy to use.
Brief description of the drawings
Fig. 1 is the fundamental diagram of gas chromatograph vacuum sampling device of the invention；
In figure, the 1. sample air valve of 2. shuttle of calibrating gas gas cylinder, 3. pressure-reducing valve, 4. filter, 5. gas valve 6.
7. the pressure sensor valve of 8. temperature sensor of temperature display meter, 9. pressure display instrument table, 10. pressure sensor 11.
The vacuum display instrument 17. of 12. gas chromatograph, 13. atmospheric valve, 14. vacuum meter valve, 15. vacuum meter 16. is vacuumized
The housing of 18. vavuum pump of valve 19..
Specific embodiment
The present invention is further described with reference to the accompanying drawings and examples.
As shown in figure 1, a kind of gas chromatograph of the invention includes calibrating gas gas cylinder 1, sample with vacuum sampling device
Container 2, gas chromatograph 12 and vavuum pump 18, calibrating gas gas cylinder 1 and shuttle 2 by tracheae respectively with gas chromatograph
12 air inlet connection, vavuum pump 18 is connected by tracheae with the exhaust outlet of gas chromatograph 12；It is also equipped with temperature sensor
8, measuring environment temperature value, temperature value passes through the reading of temperature display meter 7；Connected by pressure sensor valve 11 on described tracheae
Pressure sensor 10 is connected to, endotracheal atmospheric pressure value is measured, atmospheric pressure value passes through the reading of pressure display instrument table 9；On described tracheae
Vacuum meter 15 is connected with by vacuum meter valve 14, endotracheal vacuum is measured, vacuum passes through the reading of vacuum display instrument 16；
Atmospheric valve 13 is connected with the exhaust outlet of described gas chromatograph 12.
Being installed in series between described calibrating gas gas cylinder 1 and tracheae has pressure-reducing valve 3 and gas valve 5.
Being installed in series between described shuttle 2 and tracheae has filter 4 and sample air valve 6.
Being installed in series between described vavuum pump 18 and tracheae has vacuum pumping valve 17 and bellows.
The stainless steel tube is selected from the 316L stainless steel tubes of a diameter of 1/8in with specific reference to needs.
Described vacuum meter 15 is diagram vacuum gauge, and vavuum pump 18 is dry vacuum pump, but not limited to this can select it
Its species vacuum meter and vavuum pump.
The air inlet pipe of described gas chromatograph 12 and the overall leakage rate of blast pipe are less than or equal to 10-7Pa·m3/s。
Described gas chromatograph vacuum sampling device also includes a housing 19, described temperature sensor 8, pressure
Sensor valve 11 and vacuum meter 15 are installed on inside described housing 19；Described temperature display meter 7, pressure display instrument table 9,
Vacuum display instrument 16, pressure sensor valve 11, vacuum meter 15, atmospheric valve 13, gas valve 5, sample air valve 6 and vacuum pumping valve 17 are pacified
Loaded on the described front panel of housing 19；Described temperature display meter 7, pressure display instrument table 9 and vacuum display instrument 16
Power line is integrated into the power switch of described housing 19.
Described gas valve 5, sample air valve 6, pressure sensor valve 11, vacuum meter valve 14, vacuum pumping valve 17 and atmospheric valve 13
It is bellows valve, but not limited to this, other species valves can be selected.
Embodiment 1
A helium sample gas tank is taken, on the position of shuttle 2, during measurement obtains helium sample in accordance with the following steps
Each impurity composition volumetric concentration.
1a. opens the power switch of housing 19, pressure sensor valve 11, vacuum meter valve 14 is opened, from pressure display instrument table
9th, atmospheric pressure value, vacuum and temperature value are obtained on vacuum display instrument 16 and temperature display meter 7, temperature value is 19.9 DEG C；
1b. closes gas valve 5, vacuum pumping valve 17 and atmospheric valve 13；
1c. starts vavuum pump 18, and vacuum pumping valve 17 and sample air valve 6 are opened successively, starts to vacuumize；
1d. closes vacuum pumping valve 17 after the reading of vacuum display instrument 16 is less than 5Pa, opens shuttle 2 and switchs needed for
Sample gas enter tracheae after close shuttle 2 switch, be again turned on vacuum pumping valve 17 and vacuumize；
The process of 1e. repeat steps 9d 5-10 times；
1f. opens shuttle 2 and switchs, and according to the reading of pressure display instrument table 9, regulation shuttle 2 is switched and sample air valve 6,
Until after the reading of pressure display instrument table 9 reaches 102kPa, closing shuttle 2 and switching；
1g. measures analysis sample gas by gas chromatograph 12, and the volumetric concentration for obtaining each component is H2：2.78ppm、O2：
5.02ppm、N2：4.96ppm.
Embodiment 2
A Balance Air is taken for He, component is the calibrating gas gas cylinder of 5ppmH2,6.1ppmO2,7.5ppmN2, installed in standard
On the position of gas cylinders 1, measurement in accordance with the following steps obtains the peak area of each component chromatographic peak in calibrating gas.
2a. opens the power switch of housing 19, pressure sensor valve 11, vacuum meter valve 14 is opened, from pressure display instrument table
9th, atmospheric pressure value, vacuum and temperature value are obtained on vacuum display instrument 16 and temperature display meter 7, temperature value is 19.9 DEG C；
2b. closes sample air valve 6 and vacuum pumping valve 17, open calibrating gas gas cylinder 1 switch, gas valve 5 and atmospheric valve 13, regulation subtracts
Pressure valve 3,3-5min is purged using calibrating gas；
2c close gas valve 5 and atmospheric valve 13, start vavuum pump 18, open vacuum pumping valve 17, start to vacuumize；
2d. closes vacuum pumping valve 17 after the reading of vacuum display instrument 16 is less than 5Pa, opens gas valve 5, adjusts pressure-reducing valve 3,
Until the reading of pressure display instrument table 9 closes gas valve 5 after reaching about 100kPa, it is again turned on vacuum pumping valve 17 and vacuumizes；
The process of 2e. repeat steps d 5-10 times；
2f. opens gas valve 5 and switchs, and according to the reading of pressure display instrument table 9, pressure-reducing valve 3 is adjusted, until pressure display instrument table 9
Stable reading after 102kPa, close gas valve 5；
2g. measures analytical standard gas by gas chromatograph 12, and the peak area of each component chromatographic peak is H2：316255 μV•s、
O2：1037798μV•s、N2：1067142μV•s.
Embodiment 3
The present embodiment is essentially identical with the implementation method of embodiment 2, differs primarily in that, it is considered in the air that measurement process is subject to
The interference of oxygen nitrogen, measures oxygen and nitrogen content in high-purity helium of the purity higher than 99.999%.It is higher than 99.999% to take a purity
High-pure helium gas cylinder, on the position of calibrating gas gas cylinder 1, measurement analysis oxygen and nitrogen content is obtained present in measuring process
Background oxygen nitrogen volumetric concentration is O2：0.06ppm、N2：0.25ppm.
Claims (8)
1. a kind of gas chromatograph vacuum sampling device, it is characterised in that the device includes calibrating gas gas cylinder（1）, sample
Container（2）, gas chromatograph（12）And vavuum pump（18）, calibrating gas gas cylinder（1）And shuttle（2）By tracheae respectively with
Gas chromatograph（12）Air inlet connection, vavuum pump（18）By tracheae and gas chromatograph（12）Exhaust outlet connection；Also
Temperature sensor is installed（8）, measuring environment temperature value, temperature value is by temperature display meter（7）Reading；On described tracheae
By pressure sensor valve（11）It is connected with pressure sensor（10）, endotracheal atmospheric pressure value is measured, atmospheric pressure value is aobvious by pressure
Show instrument（9）Reading；Pass through vacuum meter valve on described tracheae（14）It is connected with vacuum meter（15）, measure endotracheal vacuum
Degree, vacuum passes through vacuum display instrument（16）Reading；Described gas chromatograph（12）Exhaust outlet on be connected with atmospheric valve
（13）.
2. gas chromatograph according to claim 1 vacuum sampling device, it is characterised in that described calibrating gas gas
Bottle（1）Being installed in series and tracheae between has pressure-reducing valve（3）With gas valve（5）.
3. gas chromatograph according to claim 1 vacuum sampling device, it is characterised in that described shuttle
（2）Being installed in series and tracheae between has filter（4）With sample air valve（6）.
4. gas chromatograph according to claim 1 vacuum sampling device, it is characterised in that described vavuum pump（18）
Being installed in series and tracheae between has vacuum pumping valve（17）And bellows.
5. gas chromatograph according to claim 1 vacuum sampling device, it is characterised in that described tracheae is stainless
Steel pipe, vacuum meter（15）It is diagram vacuum gauge, vavuum pump（18）It is dry vacuum pump.
6. gas chromatograph according to claim 1 vacuum sampling device, it is characterised in that described gas chromatograph
（12）Air inlet pipe and blast pipe overall leakage rate be less than or equal to 10-7Pa·m3/s。
7. the gas chromatograph vacuum sampling device according to claim 1,2,3 or 4, it is characterised in that also including
Individual housing（19）, described temperature sensor（8）, pressure sensor valve（11）And vacuum meter（15）It is installed on described housing
（19）It is internal；Described temperature display meter（7）, pressure display instrument table（9）, vacuum display instrument（16）, pressure sensor valve
（11）, vacuum meter（15）, atmospheric valve（13）, gas valve（5）, sample air valve（6）And vacuum pumping valve（17）It is installed on described housing
（19）Front panel；Described temperature display meter（7）, pressure display instrument table（9）With vacuum display instrument（16）Power line
It is integrated into described housing（19）Power switch.
8. the gas chromatograph vacuum sampling device according to claim 1,2,3 or 4, it is characterised in that described mark
Air valve（5）, sample air valve（6）, pressure sensor valve（11）, vacuum meter valve（14）, vacuum pumping valve（17）And atmospheric valve（13）It is ripple
Line pipe valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710028251.4A CN106706816A (en) | 2017-01-16 | 2017-01-16 | Vacuum sampling device for gas chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710028251.4A CN106706816A (en) | 2017-01-16 | 2017-01-16 | Vacuum sampling device for gas chromatograph |
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| Publication Number | Publication Date |
|---|---|
| CN106706816A true CN106706816A (en) | 2017-05-24 |
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ID=58908387
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710028251.4A Pending CN106706816A (en) | 2017-01-16 | 2017-01-16 | Vacuum sampling device for gas chromatograph |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220758A (en) * | 2019-10-25 | 2020-06-02 | 大唐水电科学技术研究院有限公司 | Remote control analysis system for gas chromatographic analysis of transformer oil |
| CN111474284A (en) * | 2020-04-09 | 2020-07-31 | 中国工程物理研究院材料研究所 | Feed gas pretreatment and automatic sample introduction system for gas chromatography |
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| EP1764603A1 (en) * | 2005-09-20 | 2007-03-21 | AC Analytical Controls Holding B.V. | Sampler system |
| CN201983961U (en) * | 2011-03-25 | 2011-09-21 | 昆明醋酸纤维有限公司 | Negative pressure sampling analytical system for gas analyzer |
| US20120118144A1 (en) * | 2010-11-12 | 2012-05-17 | Meadoworks, Inc. | Vacuum Chromatography Gas Detector |
| CN104407089A (en) * | 2014-12-09 | 2015-03-11 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Rock degassing high-sensitivity gas chromatography-mass spectrometry coupling analysis system and use method thereof |
| CN104865354A (en) * | 2015-06-09 | 2015-08-26 | 陕西省计量科学研究院 | Formaldehyde gas detector verification device, system and method |
| CN205138941U (en) * | 2015-11-24 | 2016-04-06 | 重庆大学 | Experimental device for heterogeneous attitude CO2 adsorbs desorption to big rock specimen |
| CN206420834U (en) * | 2017-01-16 | 2017-08-18 | 中国工程物理研究院核物理与化学研究所 | A kind of gas chromatograph vacuum sampling device |
-
2017
- 2017-01-16 CN CN201710028251.4A patent/CN106706816A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1764603A1 (en) * | 2005-09-20 | 2007-03-21 | AC Analytical Controls Holding B.V. | Sampler system |
| US20120118144A1 (en) * | 2010-11-12 | 2012-05-17 | Meadoworks, Inc. | Vacuum Chromatography Gas Detector |
| CN201983961U (en) * | 2011-03-25 | 2011-09-21 | 昆明醋酸纤维有限公司 | Negative pressure sampling analytical system for gas analyzer |
| CN104407089A (en) * | 2014-12-09 | 2015-03-11 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Rock degassing high-sensitivity gas chromatography-mass spectrometry coupling analysis system and use method thereof |
| CN104865354A (en) * | 2015-06-09 | 2015-08-26 | 陕西省计量科学研究院 | Formaldehyde gas detector verification device, system and method |
| CN205138941U (en) * | 2015-11-24 | 2016-04-06 | 重庆大学 | Experimental device for heterogeneous attitude CO2 adsorbs desorption to big rock specimen |
| CN206420834U (en) * | 2017-01-16 | 2017-08-18 | 中国工程物理研究院核物理与化学研究所 | A kind of gas chromatograph vacuum sampling device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220758A (en) * | 2019-10-25 | 2020-06-02 | 大唐水电科学技术研究院有限公司 | Remote control analysis system for gas chromatographic analysis of transformer oil |
| CN111474284A (en) * | 2020-04-09 | 2020-07-31 | 中国工程物理研究院材料研究所 | Feed gas pretreatment and automatic sample introduction system for gas chromatography |
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Application publication date: 20170524 |