CN210720291U - Gas chromatograph for measuring oxygen concentration by hydrogen flame ionization detector - Google Patents
Gas chromatograph for measuring oxygen concentration by hydrogen flame ionization detector Download PDFInfo
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- CN210720291U CN210720291U CN201921088892.XU CN201921088892U CN210720291U CN 210720291 U CN210720291 U CN 210720291U CN 201921088892 U CN201921088892 U CN 201921088892U CN 210720291 U CN210720291 U CN 210720291U
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Abstract
The utility model relates to a survey oxygen concentration's gas chromatograph, wherein, include: the device comprises a six-way valve, a quantitative ring and a hydrogen flame ionization detector, wherein the quantitative ring is arranged between a second interface and a fifth interface of the six-way valve; and a fourth interface of the six-way valve is connected with the hydrogen flame ionization detector. The gas chromatograph can be widely applied to monitoring the oxygen concentration in the process or the process in real time, in particular to monitoring a fixed pollution source or volatile organic compounds in the ambient air.
Description
Technical Field
The utility model discloses relate to the field of detection generally, concretely relates to utilize hydrogen flame ionization detector to survey gas chromatograph of oxygen concentration.
Background
The oxygen element is the most common simple substance form, and is the element which is most widely distributed and has the highest abundance in nature. Oxygen, colorless and odorless gas, is present in the air at a ratio of about 20.9%.
The oxidation of hydrocarbons, the treatment of wastewater, rocket propellants and the respiration of animals and humans in aviation, aerospace and diving all require oxygen. Animal respiration, combustion, and all oxidative processes (including organic matter decay) consume oxygen. In cutting and welding of metals, high purity oxygen is required to be mixed with combustible gas to generate extremely high temperature flames to melt the metals. High-purity oxygen is blown in the smelting process, so that the carbon content of the steel is reduced, impurities are removed, and combustion is maintained. In the volatile organic matter treatment, tail gas is introduced into a combustion tower, and the organic matter in the sample is combusted by adopting an oxidation and combustion treatment method to produce CO2 and water so as to reduce the air pollution caused by the organic matter.
For any process or process involving oxygen, the concentration of oxygen affects or feeds back into the overall process, even safety concerns. Therefore, real-time monitoring of oxygen concentration is particularly important.
At present, the technologies for on-line monitoring of oxygen concentration mainly include a Thermal Conductivity Detector (TCD) method of a gas chromatograph, a Pulse Discharge Helium Ionization Detector (PDHID) method of a gas chromatograph, an oxygen sensor method, and the like.
The TCD detector belongs to a concentration type detector with medium sensitivity, has poor environment interference resistance, and is very important for trace or even trace component detection; the PDHID detector has strict requirements on carrier gas and external environment, the actual operation difficulty is high, and the technical maturity is not high; the oxygen sensor (zirconia analyzer) method has strict requirements on external environmental conditions, a limited range of measurement, poor selectivity on gas or smell, dispersion of element parameters, unsatisfactory stability, high power and the like, which directly affect the accuracy of a detection result.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a method for determining oxygen concentration and gas chromatograph thereof.
The utility model provides a survey oxygen concentration's gas chromatograph, wherein, include: the device comprises a six-way valve, a quantitative ring and a hydrogen flame ionization detector, wherein the quantitative ring is arranged between a second interface and a fifth interface of the six-way valve; and a fourth interface of the six-way valve is connected with the hydrogen flame ionization detector.
Optionally, the gas chromatograph further includes: and the fourth interface of the six-way valve is connected with the hydrogen flame ionization detector through the chromatographic column. Preferably, the chromatographic column stationary phase is selected from one or more of alumina, molecular sieve, silica gel, carbon and polymer porous beads.
Optionally, the gas chromatograph further comprises a gas source unit, wherein the gas source unit is connected to the six-way valve and the hydrogen flame ionization detector.
Optionally, the gas chromatograph further comprises a control unit, wherein the control unit is connected with the six-way valve and the hydrogen flame ionization detector.
Optionally, the gas chromatograph further comprises a data processing unit, configured to receive data detected by the hydrogen flame ionization detector, and calculate and output an oxygen concentration of the sample gas according to the data.
The utility model discloses utilize hydrogen flame ionization detector to survey oxygen concentration, hydrogen Flame Ionization Detector (FID) detects to the organic matter, is a general type detector of high sensitivity, and sensitivity is high, exceeds nearly 3 orders of magnitude than the thermal conductivity detector, detects the lower limit and can hang down to 10-13g/s, linear range as wide as 107-1012The detector has the advantages of simple structure, good stability, high sensitivity and quick response, has a certain response signal for detecting oxygen, and is an ideal detector.
The utility model discloses a but gas chromatograph wide application in real-time supervision technology or in-process oxygen concentration's size, especially to the monitoring of fixed pollution source or ambient air volatility organic matter.
Drawings
Fig. 1 is a diagram of an embodiment of a gas chromatograph according to the present invention;
fig. 2 shows an embodiment of the gas chromatograph according to the present invention.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, so that the aspects of the invention and their advantages can be better understood. However, the specific embodiments and examples described below are for illustrative purposes only and are not intended to limit the present invention.
The execution sequence of each step in the method of the present invention is not limited to the sequence presented in the text unless otherwise specified, that is, the execution sequence of each step can be changed, and other steps can be inserted between two steps as required.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "connected" and "disposed" are to be understood in a broad sense, for example, either fixedly or detachably or integrally: may be mechanically connected, may be electrically connected or may be in communication with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. In order to simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or reference letters in the various examples, which have been repeated for purposes of simplicity and clarity and do not in themselves dictate a relationship between the various embodiments and/or arrangements discussed. In addition, the present disclosure provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or use of other materials.
In some embodiments of the present invention, a method for determining oxygen concentration using a hydrogen flame ionization detector comprises:
calibrating an instrument: concentration C by hydrogen flame ionization detectorO2Peak area A corresponding to oxygen standard gasO2And retention time RTO2. Wherein the retention time RTO2The method is used for performing qualitative determination on chromatographic peaks to judge whether the chromatographic peaks are oxygen peaks, and the accurate determination is a precondition for calculating the oxygen concentration.
And (3) analysis: determining the peak area A corresponding to the oxygen component in the sample gas by the hydrogen flame ionization detectori。
Data processing: the oxygen component concentration C in the sample gas was calculated by the following formulai，
Ci＝CO2·Ai/AO2。
The hydrogen Flame Ionization Detector (FID) is a high-sensitivity universal detector for detecting organic matters, has high sensitivity which is higher than that of a thermal conductivity detector by nearly 3 orders of magnitude, and the lower detection limit can be as low as 10-13g/s, linear range as wide as 107～1012The detector has the advantages of simple structure, good stability, high sensitivity and quick response, has a certain response signal for detecting oxygen, and is an ideal detector.
In view of a certain response signal of oxygen with a certain concentration on the FID, oxygen peaks with different peak area sizes are generated, and the retention time is consistent. Therefore, a relational expression between the oxygen peak area and the corresponding oxygen concentration can be established. By the quantitative relation between the oxygen peak area and the oxygen concentration, the oxygen concentration in the process or the process can be monitored in real time according to the oxygen peak area in the gas chromatogram so as to feed back the real-time oxygen concentration in the environment or the working condition.
In some embodiments, the analyzing further comprises separating the oxygen component. Specifically, the separating the oxygen component includes passing the sample gas through a chromatographic column to separate the oxygen component from other components.
The chromatographic column stationary phase is selected from one or more of alumina, molecular sieve, silica gel, carbon and polymer porous beads.
In some embodiments, the oxygen standard gas concentration ranges from 0-21% and is not 0.
In some embodiments, during the instrument calibration and the analysis steps, the combustion gas is hydrogen, the combustion supporting gas is hydrocarbon-depleted air, and the carrier gas is nitrogen. The flow ratio range of the combustion-supporting gas and the combustion gas is 6-11. The flow range of the combustion-supporting gas is (320-500) mL/min.
The method for measuring the oxygen concentration by using the hydrogen flame ionization detector can be widely applied to monitoring the oxygen concentration in a process or a process in real time, and especially can be used for monitoring a fixed pollution source or volatile organic compounds in ambient air.
On the basis of Volatile Organic Compounds (VOCs) monitoring sites, chromatographic peaks including total hydrocarbon and oxygen peaks can be detected by FID in each monitoring period. By calculating the oxygen peak area of the obtained chromatogram, the real-time oxygen concentration in the sample can be monitored. The oxygen concentration monitoring by adopting the existing on-line FID is not only significant, but also easy to realize. The oxygen peak and chromatographic peaks such as total hydrocarbons and the like can be obtained in the same period, and only the oxygen peak in the obtained chromatographic spectrum needs to be processed, so that additional hardware equipment does not need to be added.
In some embodiments of the present invention, as shown in fig. 1, a gas chromatograph for measuring oxygen concentration by the above method comprises: a six-way valve 1, a quantitative ring 2, a chromatographic column 3 and a hydrogen flame ionization detector 4. A quantitative ring is arranged between the second connector 12 and the fifth connector 15 of the six-way valve 1. The fourth interface 14 of the six-way valve 1 is connected with the hydrogen flame ionization detector 4 through the chromatographic column 3.
In the step instrument calibration, two processes of sample introduction and test are completed through the switching of the six-way valve 1.
When the standard gas is injected, the oxygen standard gas enters from the first interface 11 (namely a sample gas inlet) of the six-way valve 1, enters the quantitative ring 2 through the second interface 12, and then sequentially leaves the six-way valve 1 through the fifth interface 15 and the sixth interface 16 (namely a sample gas outlet) of the six-way valve 1, and at the moment, the oxygen standard gas is filled in the quantitative ring 2; the carrier gas enters from the third interface 13 (i.e. carrier gas inlet) of the six-way valve 1, and enters the hydrogen flame ionization detector 4 through the fourth interface 14 of the six-way valve 1 and the chromatographic column 3.
When the standard gas is tested, the six-way valve 1 is switched from a sample injection state to a test state, at the moment, the oxygen standard gas enters from the first interface 11 of the six-way valve 1, is discharged through the sixth interface 16, the carrier gas enters from the third interface 13 of the six-way valve 1, and enters the hydrogen flame ionization detector 4 after sequentially passing through the second interface 12 of the six-way valve 1, the quantitative ring 2, the fifth interface 15 of the six-way valve 1, the fourth interface 14 and the chromatographic column 3. At this time, the carrier gas carries the oxygen standard gas in the quantitative ring into the hydrogen flame ionization detector 4 for detection.
In the step analysis, two processes of sample introduction and test are completed through the switching of the six-way valve 1.
When sample gas is fed, the sample gas enters from the first interface 11 (namely a sample gas inlet) of the six-way valve 1, enters the quantitative ring 2 through the second interface 12, and then sequentially leaves the six-way valve 1 through the fifth interface 15 and the sixth interface 16 (namely a sample gas outlet) of the six-way valve 1, and at the moment, the sample gas fills the quantitative ring 2; the carrier gas enters from the third interface 13 (i.e. carrier gas inlet) of the six-way valve 1, and enters the hydrogen flame ionization detector 4 through the fourth interface 14 of the six-way valve 1 and the chromatographic column 3.
When a sample gas is tested, the six-way valve 1 is switched from a sample introduction state to a test state, at the moment, the sample gas enters from the first interface 11 of the six-way valve 1, is discharged through the sixth interface 16, and the carrier gas enters from the third interface 13 of the six-way valve 1, sequentially passes through the second interface 12 of the six-way valve 1, the quantitative ring 2, the fifth interface 15 of the six-way valve 1, the fourth interface 14 and the chromatographic column 3, and then enters the hydrogen flame ionization detector 4. Wherein the oxygen component in the sample gas is separated from other components on the chromatographic column 3, and the carrier gas carries the oxygen component into the hydrogen flame ionization detector 4 for detection.
In some embodiments of the invention, the chromatographic column stationary phase is selected from one or more of alumina, molecular sieves, silica gel, carbon, and polymeric porous beads.
In some embodiments of the present invention, as shown in fig. 2, the gas chromatograph further comprises a gas source unit 5 and a data processing unit 6. And the gas source unit 5 is connected with the six-way valve 1 and the hydrogen flame ionization detector 4 and is used for providing combustion-supporting gas, combustion gas, carrier gas and the like. The data processing unit 6 is used for receiving the data detected by the hydrogen flame ionization detector 4, and calculating and outputting the oxygen concentration of the sample gas according to the data.
In some embodiments of the present invention, the gas chromatograph further comprises a control unit, the control unit connecting the six-way valve and the hydrogen flame ionization detector. The control unit controls the six-way valve and the hydrogen flame ionization detector to complete the oxygen concentration determination. Further, the control unit also controls other units of the gas chromatograph, such as a gas source unit, to perform the above-described oxygen concentration measurement.
Examples
The sample gas was detected by a gas chromatograph as shown in FIG. 2
The operating conditions of the instrument are as follows: the temperature of the column box is 110 ℃, the flow rate of combustion gas (hydrogen) is 40ml/min, the flow rate of combustion-supporting gas (hydrocarbon-removing air) is 320ml/min, the hydrogen-air ratio is 1:8, the flow rate of carrier gas (nitrogen) is 40ml/min, and the sample injection flow rate is 60 ml/min.
The instrument is calibrated by adopting standard gas with the oxygen concentration of 10.03 percent and the helium as the rest component.
After calibration is completed, standard gases with different concentrations are tested.
A,
The operating conditions of the instrument are as follows: the temperature of the column box is 110 ℃, the flow rate of combustion gas is 40ml/min, the flow rate of combustion-supporting gas is 320ml/min, the hydrogen-air ratio is 1:8, the flow rate of carrier gas is 40ml/min, and the flow rate of sample injection is 60 ml/min.
Concentration of sample gas: the oxygen concentration is 9.98%, and the propane concentration is 150mg/m3And the balance of nitrogen. Four measurements were made, and the results are given in the following table.
II,
The operating conditions of the instrument are as follows: the temperature of the column box is 110 ℃, the flow rate of combustion gas is 40ml/min, the flow rate of combustion-supporting gas is 320ml/min, the hydrogen-air ratio is 1:8, the flow rate of carrier gas is 40ml/min, and the flow rate of sample injection is 60 ml/min.
Concentration of sample gas: the oxygen concentration is 20.03%, and the rest is nitrogen. Four measurements were made, and the results are given in the following table.
III,
The operating conditions of the instrument are as follows: the temperature of the column box is 110 ℃, the flow rate of combustion gas is 40ml/min, the flow rate of combustion-supporting gas is 320ml/min, the hydrogen-air ratio is 1:8, the flow rate of carrier gas is 40ml/min, and the flow rate of sample injection is 60 ml/min.
Concentration of sample gas: the oxygen concentration is 20.18%, and the propane concentration is 149.8mg/m3And the balance of nitrogen. Four measurements were made, and the results are given in the following table.
According to the detection result, the utility model discloses a gas chromatograph can accurate oxygen concentration in the detected gas, and repeatability is good.
Finally, it should be noted that: it should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious changes and modifications may be made without departing from the scope of the present invention.
Claims (6)
1. A gas chromatograph for measuring an oxygen concentration, comprising: a six-way valve, a quantitative ring and a hydrogen flame ionization detector,
the quantitative ring is arranged between the second interface and the fifth interface of the six-way valve;
and a fourth interface of the six-way valve is connected with the hydrogen flame ionization detector.
2. The gas chromatograph of claim 1, further comprising: and the fourth interface of the six-way valve is connected with the hydrogen flame ionization detector through the chromatographic column.
3. The gas chromatograph of claim 2, wherein the chromatographic column stationary phase is selected from one or more of alumina, molecular sieves, silica gel, carbon, and polymeric porous beads.
4. The gas chromatograph of claim 1, further comprising a gas source unit connecting the six-way valve and the hydrogen flame ionization detector.
5. The gas chromatograph of claim 1, further comprising a control unit that connects the six-way valve and the hydrogen flame ionization detector.
6. The gas chromatograph of claim 1, further comprising a data processing unit configured to receive data detected by the hydrogen flame ionization detector and to calculate and output an oxygen concentration of the sample gas based on the data.
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| CN110376324A (en) * | 2019-07-12 | 2019-10-25 | 北京雪迪龙科技股份有限公司 | Utilize the method and gas chromatograph of flame ionization ditector measurement oxygen concentration |
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| CN110376324A (en) * | 2019-07-12 | 2019-10-25 | 北京雪迪龙科技股份有限公司 | Utilize the method and gas chromatograph of flame ionization ditector measurement oxygen concentration |
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