CN107843682B - Fault detection method for VOC waste gas continuous analysis device and VOC waste gas continuous analysis device - Google Patents
Fault detection method for VOC waste gas continuous analysis device and VOC waste gas continuous analysis device Download PDFInfo
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- CN107843682B CN107843682B CN201610829498.1A CN201610829498A CN107843682B CN 107843682 B CN107843682 B CN 107843682B CN 201610829498 A CN201610829498 A CN 201610829498A CN 107843682 B CN107843682 B CN 107843682B
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- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8637—Peak shape
Abstract
The invention provides a fault detection method of a VOC waste gas continuous analysis device, which comprises a pretreatment part and a gas chromatograph, and comprises the following steps: performing continuous analysis on the VOC sample; comparing, with respect to chromatographic peaks corresponding to target substances contained in the sample detected in a continuous analysis process, an area value and a retention time of the chromatographic peaks detected two adjacent times, respectively; and when the area value of the chromatographic peak detected at the next time in the two adjacent detected chromatographic peaks is smaller than the area value of the chromatographic peak detected at the previous time by more than a specified value, and the retention time of the chromatographic peak detected at the next time is smaller than the retention time of the chromatographic peak detected at the previous time by more than a specified value, determining that a fault occurs and outputting a fault detection signal. Also provides a continuous analysis device for VOC waste gas.
Description
Technical Field
The invention relates to the technical field of gas chromatography continuous analysis and waste gas continuous analysis, in particular to a fault detection method of a VOC waste gas continuous analysis device and the VOC waste gas continuous analysis device.
Background
The abnormalities of gas chromatography in continuous analysis of VOC (volatile organic compound) exhaust gas using a gas chromatograph are generally classified into two major categories, relating to the shape of peaks and relating to baselines. As the peak shape abnormality, various phenomena such as smear distortion, leading, peak breakage, retention time variation, undetected peak, small peak as a whole, ghost peak/left, and the like generally occur. For example, fig. 1 shows several common phenomena of abnormal peak shape, in which (a) indicates a peak breakage phenomenon, (b) indicates a small peak phenomenon, and (c) indicates an advance phenomenon.
When gas chromatography analysis is performed in a laboratory or the like, the above-described abnormality of the gas chromatography may occur due to: (1) the test conditions (analysis conditions) matched with the sample adjusted by the user for the VOC exhaust gas continuous analysis apparatus are not appropriate; (2) machine failure or contamination/deterioration occurs in the VOC exhaust gas continuous analysis apparatus. Therefore, by studying the abnormality of the peak shape of the chromatographic peak due to the adjustment of the test conditions by the user or the trouble or the contamination/degradation of the device and designing a means for detecting the abnormality/trouble occurring in the VOC exhaust gas continuous analyzer based on the chromatographic information obtained by the chromatographic analysis, it is possible to deal with the abnormality existing in the VOC exhaust gas continuous analyzer at an early stage and prevent the problem in advance.
Disclosure of Invention
The VOC exhaust gas continuous analysis apparatus using a gas chromatograph includes a gas chromatograph and a pretreatment section for introducing a sample gas into the gas chromatograph.
In the continuous analysis of VOC exhaust gas, since the target substance of the sample to be measured and the measurement condition are known in advance, the gas chromatograph is shipped in an adjusted state, and therefore, in general, abnormality of the gas chromatograph due to the analysis condition adjusted by the user does not occur, but trouble of the gas chromatograph due to machine trouble or contamination/deterioration occurs. Conventionally, a gas chromatograph used for continuous analysis of VOC exhaust gas has a function of automatically detecting an analyzer abnormality such as leakage from a solenoid valve of an analysis unit of the gas chromatograph and flame reduction of an FID detector.
However, in the continuous analysis of VOC exhaust gas, there is no detection of abnormality or trouble in the equipment for sampling the samples in the pretreatment section due to machine trouble or contamination/deterioration. Since the abnormality or failure of the sampling device in the preprocessing section causes the abnormality of the peak shape in the gas chromatography analysis, it is necessary to investigate the cause of the abnormality or failure in the preprocessing section from the peak shape of the gas chromatography, and to investigate a countermeasure capable of detecting the abnormality or failure in the preprocessing section so as to prevent the failure in advance.
In view of the above problems, an object of the present invention is to provide a method for detecting a malfunction of a VOC exhaust gas continuous analysis apparatus. With the malfunction detection method for the VOC exhaust gas continuous analyzer, it is possible to detect a malfunction of the pretreatment unit of the VOC exhaust gas continuous analyzer in the VOC exhaust gas continuous analysis, and thus it is possible to deal with the malfunction early and restart the normal operation again.
Another object of the present invention is to provide a continuous analysis apparatus for VOC exhaust gas. The continuous analysis device for VOC exhaust gas can detect the fault of the pretreatment part in the continuous analysis of VOC exhaust gas, thereby treating the fault early and restarting the normal operation.
According to an aspect of the present invention, there is provided a method of detecting a malfunction of a VOC exhaust gas continuous analysis apparatus including a preprocessing section and a gas chromatograph, the method including: performing continuous analysis on the VOC sample; comparing, with respect to chromatographic peaks corresponding to target substances contained in the sample detected in a continuous analysis process, an area value and a retention time of the chromatographic peaks detected two adjacent times, respectively; and when the area value of the chromatographic peak detected at the next time in the two adjacent detected chromatographic peaks is smaller than the area value of the chromatographic peak detected at the previous time by more than a specified value, and the retention time of the chromatographic peak detected at the next time is smaller than the retention time of the chromatographic peak detected at the previous time by more than a specified value, determining that a fault occurs and outputting a fault detection signal.
Further, according to the malfunction detection method of the VOC exhaust gas continuous analysis apparatus described above, if the gas chromatograph is determined to have a malfunction before the VOC sample is continuously analyzed, the gas chromatograph is adjusted to remove the malfunction.
Further, according to the failure detection method of the VOC exhaust gas continuous analysis apparatus described above, the determining that the failure occurs includes determining that the preprocessing section has a failure.
According to another aspect of the present invention, there is provided a VOC exhaust gas continuous analysis apparatus including a pretreatment section and a gas chromatograph, the VOC exhaust gas continuous analysis apparatus further including: a fault detection section including: a comparison unit that compares, with respect to a chromatographic peak corresponding to a target substance contained in a VOC sample detected in a continuous analysis process of the sample, an area value and a retention time of the chromatographic peak detected twice adjacent to each other; and a failure determination unit configured to determine that a failure has occurred and output a failure detection signal when an area value of the chromatographic peak detected next to the chromatographic peak detected two adjacent times becomes smaller than an area value of the chromatographic peak detected previous by a predetermined value or more and a retention time of the chromatographic peak detected next by the predetermined value or more is smaller than a retention time of the chromatographic peak detected previous by the predetermined value or more.
Further, according to the above-described VOC exhaust gas continuous analysis apparatus, if the gas chromatograph is determined to have a malfunction before the VOC sample is continuously analyzed, the gas chromatograph is adjusted to eliminate the malfunction.
Further, according to the above-described VOC exhaust gas continuous analysis apparatus, the determining that the malfunction occurs includes determining that the preprocessing section malfunctions.
As described above, according to the method for detecting a malfunction of a VOC exhaust gas continuous analyzer and the VOC exhaust gas continuous analyzer of the present invention, it is possible to detect a malfunction of a preprocessing unit in the VOC exhaust gas continuous analyzer, to deal with the malfunction early, and to restart a normal operation to prevent the malfunction in advance.
Drawings
Other objects and further features of the embodiments will become apparent from the following detailed description when read in conjunction with the accompanying drawings, in which:
FIG. 1 illustrates several common phenomena of peak shape anomalies;
fig. 2 is a block diagram showing the main constitution of a VOC exhaust gas continuous analysis apparatus according to an embodiment of the present invention;
fig. 3 shows a flow chart relating to continuous analysis of VOC exhaust gas in accordance with an embodiment of the present invention.
Detailed Description
To further illustrate the present invention, the following description of the embodiments with reference to the accompanying drawings will be further described in detail.
Fig. 2 shows a block diagram of the main constitution of the VOC exhaust gas continuous analysis apparatus 1 according to the embodiment of the present invention. As shown in fig. 2, the VOC exhaust gas continuous analyzer 1 according to the embodiment includes a preprocessing unit 11, a gas chromatograph 12, and a failure detection unit 13. In the continuous analysis of the VOC exhaust gas, the gas chromatograph 12 constitutes an analysis section of the continuous analysis apparatus 1 for VOC exhaust gas; the pretreatment unit 11 is configured to mount a pump at the rear stage of the gas chromatograph 12, and to suck and sample the VOC exhaust gas; the failure detection unit 13 is used for failure detection in the VOC continuous analysis, and includes a comparison unit 131 and a failure determination unit 132, and the failure detection unit 13 may be realized by an algorithm incorporated in the VOC exhaust gas continuous analysis device 1.
In the VOC exhaust gas continuous analyzer 1 shown in fig. 2, a sample is sampled under negative pressure. In order to sample a sample under negative pressure, the atmospheric pressure was equalized before the start of the analysis. In general, it is important to perform stable continuous analysis in which the sampled sample gas is made to have a certain volume.
However, when the pre-processing section 11 fails, for example, the atmospheric pressure balance at the time of sampling the sample may be lost due to a failure of the electromagnetic valve of the pre-processing section 11, a blockage of the flow path of the pre-processing section 11, or a failure of the pump. On the other hand, when the atmospheric pressure equilibrium is lost, the retention time of the peak shape of the chromatographic peak detected by analyzing the sample is changed (shortened), and the retention time is changed (shortened), and the peak shape is also reduced.
The inventors of the present invention have studied the change of the chromatographic peak when the pre-processing section 11 is faulty, and then have proposed a fault detection method for the pre-processing section 11 of the VOC exhaust gas continuous analyzer 1 based on the chromatographic information. By using this failure detection method, it is possible to implement a self-detection function of abnormality/failure in the preprocessing unit 11 in the VOC exhaust gas continuous analysis, and it is possible to deal with the abnormality/failure in the preprocessing unit 11 at an early stage and restart normal operation to prevent failure in advance.
The main idea of the fault detection method of the VOC waste gas continuous analysis device is as follows: when the area value of a detected chromatographic peak corresponding to a target substance (for example, methane) contained in a VOC sample is smaller than the area value of a chromatographic peak measured immediately before by a predetermined value or more and the retention time of the detected chromatographic peak is smaller than the retention time of the chromatographic peak measured immediately before by a predetermined value or more in continuous analysis of the VOC sample (exhaust gas sampling), it is automatically determined that a failure has occurred in the preprocessing unit and a failure detection signal is output. The "predetermined value" referred to herein is settable and can be set based on experience of a change in a chromatographic peak that would normally occur when a failure occurs in the pre-processing section.
Therefore, the method for detecting the malfunction of the VOC exhaust gas continuous analysis apparatus according to the present invention mainly comprises: performing continuous analysis on the VOC sample; comparing the area value and retention time of two adjacent chromatographic peaks corresponding to the target substance contained in the sample, which are detected in the continuous analysis process, respectively; and when the area value of the chromatographic peak detected at the next time in the two adjacent detected chromatographic peaks is smaller than the area value of the chromatographic peak detected at the previous time by more than a specified value and the retention time of the chromatographic peak detected at the next time is smaller than the retention time of the chromatographic peak detected at the previous time by more than a specified value, judging that a fault occurs and outputting a fault detection signal.
In the VOC exhaust gas continuous analyzer 1 shown in fig. 2, the failure detection unit 13 is configured to detect a failure in the VOC continuous analysis, wherein the comparison unit 131 is configured to perform comparison between an area value and a retention time of a two-adjacent detected chromatographic peak with respect to a chromatographic peak corresponding to a target substance included in a sample detected in the continuous analysis, and the failure determination unit 132 is configured to determine that a failure has occurred and output a failure detection signal when an area value of a next detected chromatographic peak among two-adjacent detected chromatographic peaks is smaller by a predetermined value or more from an area value of a previously detected chromatographic peak and a retention time of a next detected chromatographic peak is smaller by a predetermined value or more from a retention time of a previously detected chromatographic peak.
As described above, the method for detecting a malfunction in a VOC exhaust gas continuous analyzer according to the present invention mainly determines whether or not an abnormality or malfunction occurs in a preprocessing section of the VOC exhaust gas continuous analyzer by comparing two adjacent chromatographic peaks detected during continuous analysis of a VOC sample. Therefore, in order to ensure the accuracy of detecting the abnormality/fault of the pretreatment unit by using the fault detection method of the VOC exhaust gas continuous analysis device, there should be no abnormality in the first chromatographic peak detected when the VOC sample is continuously analyzed, that is, there should be no fault in the VOC exhaust gas continuous analysis device before the VOC sample is continuously analyzed in the fault detection method, otherwise the fault detection of the VOC exhaust gas continuous analysis device is inaccurate.
As described above, the malfunction that may occur in the VOC exhaust gas continuous analysis apparatus 1 includes the malfunction of the gas chromatograph 12 and the malfunction of the preprocessing unit 11. Since the gas chromatograph 12 generally used for continuous analysis of VOC exhaust gas has a self-abnormality detection function, a trouble of the gas chromatograph 12 can be checked by the self-abnormality detection function of the gas chromatograph 12. The troubleshooting by the preprocessing unit 11 is specifically described below with reference to fig. 3.
Fig. 3 shows a flow chart relating to continuous analysis of VOC exhaust gas in accordance with an embodiment of the present invention.
First, in step S101, it is determined whether the gas chromatograph 12 has detected itself as a failure/abnormality. When the gas chromatograph 12 is determined that there is a malfunction therein, that is, that a malfunction detection signal is output (yes in step S101), the gas chromatograph 12 needs to be adjusted to eliminate the malfunction (step S102). Here, when any other step in fig. 3 is performed, the flow returns to step S101 whenever the gas chromatograph 12 detects by itself that a failure/abnormality has occurred, that is, a failure detection signal is output.
When there is no failure in the gas chromatograph 12, that is, no failure detection signal is output (no in step S101), next, in step S103, it is determined whether or not a failure is detected in the preprocessing unit 11 in the process of the previous continuous exhaust gas analysis. If the preprocessing unit 11 is determined to have a failure in step S103 (yes in step S103), the preprocessing unit 11 is adjusted to eliminate the failure (step S104). Here, the determination in step S103 may be performed by the failure determination unit 132, for example. Since the failure determination unit 132 is used to determine whether or not a failure has occurred in the preprocessing unit 11 in the process of the previous continuous exhaust gas analysis, it is convenient to perform the determination by using the failure determination unit 132 in step S103. Of course, other means may be used to perform the determination in step S103, and the present invention is not limited herein. Here, if the VOC exhaust gas continuous analysis device 1 is not used to perform the continuous exhaust gas analysis before the continuous exhaust gas analysis is currently started, it is determined in step S103 that there is no failure in the preprocessing unit 11, because the VOC exhaust gas continuous analysis device 1 is subjected to the installation and debugging before being used to perform the continuous exhaust gas analysis, and it can be ensured that no failure occurs when the first continuous exhaust gas analysis is performed.
Next, when it is determined in step S103 that there is no failure in the preprocessing unit 11 (no in step S103), in step S105, continuous analysis of the VOC sample currently sampled is started. As described above, by the steps S101 and S103, it is possible to ensure that there is no trouble in the VOC exhaust gas continuous analysis apparatus 1 before the present continuous analysis of the VOC samples, thereby ensuring the accuracy of the detection of abnormality/trouble in the preprocessing section 11 in the VOC exhaust gas continuous analysis.
Next, in step S106, the chromatographic peaks corresponding to the target substance contained in the sample detected in the continuous exhaust gas analysis process in step S105 are compared with the area value and retention time of the chromatographic peaks detected two adjacent times.
Then, in step S107, it is determined whether or not the area value of the chromatographic peak detected next to the chromatographic peak detected two adjacent times is smaller than the area value of the chromatographic peak detected previous time by a predetermined value or more and the retention time of the chromatographic peak detected next time is smaller than the retention time of the chromatographic peak detected previous time by a predetermined value or more, based on the result in step S106. If the area value of the chromatographic peak detected next to the chromatographic peak detected two adjacent times becomes smaller than the area value of the chromatographic peak detected last by a predetermined value or more and the retention time of the chromatographic peak detected next becomes smaller than the retention time of the chromatographic peak detected last by a predetermined value or more, the failure determination unit 132 determines that the preprocessing unit 11 has failed and outputs a failure detection signal. When the preprocessing unit 11 is determined to have a failure during the continuous exhaust gas analysis, in order to ensure the accuracy of the analysis, it is necessary to stop the current continuous exhaust gas analysis and to remove the failure of the preprocessing unit 11 so as to start the next continuous exhaust gas analysis.
Therefore, the flow returns to step S103, and the preprocessing unit 11 is determined to be malfunctioning in step S103 (yes in step S103). At this time, the preprocessing unit 11 is adjusted to eliminate the failure of the preprocessing unit 11 (step S104), so that the normal operation of the VOC exhaust gas continuous analyzer 1 can be recovered as soon as possible.
As described above, according to the method for detecting a malfunction of a VOC exhaust gas continuous analyzer and the VOC exhaust gas continuous analyzer provided by the present invention, it is possible to detect a malfunction of a preprocessing unit in the VOC exhaust gas continuous analyzer, to deal with the malfunction at an early stage, and to restart normal operation to prevent the malfunction in the future.
While the present invention has been described in conjunction with specific embodiments, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended that such alternatives, modifications, and variations be included within the spirit and scope of the appended claims.
Claims (4)
1. A method for detecting a malfunction of a VOC exhaust gas continuous analyzer, the VOC exhaust gas continuous analyzer comprising a preprocessing unit and a gas chromatograph, the method comprising:
performing continuous analysis on the VOC sample;
comparing, with respect to chromatographic peaks corresponding to target substances contained in the sample detected in a continuous analysis process, an area value and a retention time of the chromatographic peaks detected two adjacent times, respectively; and
and when the area value of the chromatographic peak detected at the next time in the two adjacent detected chromatographic peaks is smaller than the area value of the chromatographic peak detected at the previous time by more than a specified value, and the retention time of the chromatographic peak detected at the next time is smaller than the retention time of the chromatographic peak detected at the previous time by more than a specified value, the preprocessing unit judges that a fault occurs and outputs a fault detection signal.
2. A method for detecting malfunction of an apparatus for continuous analysis of VOC exhaust gas as claimed in claim 1,
adjusting the gas chromatograph to troubleshoot the malfunction if the gas chromatograph is determined to be malfunctioning prior to continuously analyzing the VOC sample.
3. The continuous VOC waste gas analysis device is characterized by comprising a pretreatment part and a gas chromatograph, and further comprising:
a fault detection section including:
a comparison unit that compares, with respect to a chromatographic peak corresponding to a target substance contained in a VOC sample detected in a continuous analysis process of the sample, an area value and a retention time of the chromatographic peak detected twice adjacent to each other; and
and a failure determination unit configured to determine that the preprocessing unit has failed and output a failure detection signal when an area value of the chromatographic peak detected next to the chromatographic peak detected two adjacent times becomes smaller than an area value of the chromatographic peak detected previous time by a predetermined value or more and a retention time of the chromatographic peak detected next time becomes smaller than a retention time of the chromatographic peak detected previous time by a predetermined value or more.
4. A VOC exhaust gas continuous analysis apparatus as claimed in claim 3,
adjusting the gas chromatograph to troubleshoot the malfunction if the gas chromatograph is determined to be malfunctioning prior to continuously analyzing the VOC sample.
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