CN115046952B - Detection signal processing method of elemental analysis instrument and gas detection device thereof - Google Patents
Detection signal processing method of elemental analysis instrument and gas detection device thereof Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 115
- 238000000921 elemental analysis Methods 0.000 title claims abstract description 13
- 238000003672 processing method Methods 0.000 title claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims abstract description 74
- 238000011897 real-time detection Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 8
- 230000001360 synchronised effect Effects 0.000 claims description 5
- 238000002372 labelling Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001745 non-dispersive infrared spectroscopy Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/274—Calibration, base line adjustment, drift correction
- G01N21/276—Calibration, base line adjustment, drift correction with alternation of sample and standard in optical path
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention discloses a detection signal processing method of an elemental analysis instrument, which comprises the following steps: 1. one path of reference channel is added on the basis of the detection channel of the element analysis instrument; 2. labeling the detection channel baseline value as BC0 and the reference channel baseline value as BR0;3. dividing each reference channel value RS [ i ] by a reference channel base value BR0 to obtain a change coefficient KS [ i ], and dividing the detection channel base value BC0 by the change coefficient KS [ i ] to obtain a real-time detection channel base value BKS [ i ];4. subtracting the real-time detection channel baseline value BKS [ i ] from the real-time read detection channel value CS [ i ] to obtain a real-time signal integral value CI [ i ];5. and accumulating the values obtained by checking the linear table of each real-time signal integral value CI [ i ], and dividing the values by the weight of the sample to obtain the element content value in the sample. Also disclosed is a gas detection device for realizing the detection signal processing method of the element analysis instrument. The invention greatly improves the detection precision.
Description
Technical Field
The invention relates to the technical field of elemental analysis instruments, in particular to a detection signal processing method of an elemental analysis instrument and a gas detection device thereof.
Background
The elemental analysis instrument is used for analyzing the content of elements such as carbon, sulfur, oxygen and hydrogen in a material, adopts means such as heating to change the elements such as carbon, sulfur, oxygen and hydrogen in the detected material into gaseous substances (CO\CO 2\SO2\H2 O), then detects the concentration of the gaseous substances, adds up the integration to obtain the total content of carbon, sulfur, oxygen and hydrogen elements, and divides the total content by the mass of the detected material before heating to obtain the percentage content of carbon, sulfur and oxygen.
Referring to fig. 1, there is shown a conventional gas detection device for an elemental analyzer, which includes an analysis cell 10, an infrared light source 20, an infrared sensor 30, and a filter 40. The analysis chamber 10 has a gas input end 11 and a gas output end 12, and the gas input end 11 and the gas output end 12 of the analysis chamber 10 are directly communicated with the external atmosphere. An infrared light source 20 is provided at one side of the analysis gas cell 10 for infrared irradiation of the gas to be detected within the analysis gas cell 10. An infrared sensor 30 is provided at the other side of the analysis gas cell 10 for detecting the gas concentration within the analysis gas cell 10. The optical filter 40 is located between the analysis chamber 10 and the infrared sensor 40. The intensity I 0 of the infrared light emitted from the infrared light source 20, and the intensity I 1 of the infrared sensor 30 which is reduced after the detected gas is absorbed, the extinction I 1/I0 reflects the concentration of the detected gas.
The gas detection device detects the concentration of CO\CO 2\SO2\H2 O gas by using the NDIR infrared optical principle, and the instrument can cause the drift of signals of an infrared detection part due to the influence of various factors such as atmospheric pressure, ambient temperature, the impact of the detected gas temperature on an infrared detection part and the change of the infrared detection part (such as the drift of an infrared light source and the change of a light absorption coefficient caused by the pollution of an infrared light path) and the like in the use environment, wherein the drift comprises a baseline drift part and a range drift part.
For baseline drift, the current technology is to introduce pure gas (usually carrier gas) into the infrared analysis air chamber before each sample analysis, record a section of stable sensor signal value, take the average value as the baseline value BC0 of the sample analysis, and subtract the fixed baseline value BC0 from each detection signal value in the analysis process to obtain the actual detection value. This conventional method does eliminate most of baseline drift, but since this baseline value is performed before the sample is not analyzed, in practice, when the sample is analyzed, since the mixed gas of the sample released gas and the carrier gas is always in the process of changing the temperature, the pressure and the flow rate when passing through the gas chamber, it is still different from the pure gas (usually carrier gas) which is introduced in a stable state, and the analysis time is generally more than 20 seconds, during which the use environment has atmospheric pressure, the ambient temperature, the detected gas temperature impacts the infrared detection component and the change of the infrared detection component itself (such as the drift of the infrared light source, the change of the light absorption coefficient caused by the pollution of the infrared light path) and other factors cannot be guaranteed to be the same as those when detecting BC0, thereby causing the drift of the detection result.
The current technology can limit the change to a very small range through technical means such as pressure stabilization, flow stabilization and air chamber constant temperature, but still can cause certain influence on the accuracy and stability of analysis results, generally, correction is required to be carried out every shift (8 hours) to ensure the accuracy of equipment, correction is required to be carried out at any time when an edge result is met, and the quick detection performance of the instrument cannot be fully exerted, which is also the maximum difference between the technical indexes of domestic analysis instruments and international advanced analysis instruments.
To this end, the present inventors have found a method for solving the above-mentioned problems through beneficial studies and studies, and the technical solutions to be described below are made in this context.
Disclosure of Invention
One of the technical problems to be solved by the invention is as follows: aiming at the defects of the prior art, the detection signal processing method of the element analysis instrument for reducing analysis result errors caused by baseline fluctuation is provided.
The second technical problem to be solved by the invention is that: a gas detection device for realizing the detection signal processing method of the element analysis instrument is provided.
A detection signal processing method of an elemental analysis instrument as a first aspect of the present invention includes the steps of:
step S10, adding a reference channel on the basis of a detection channel of an element analysis instrument, wherein the sampling frequency of the reference channel is synchronous with the sampling frequency of the detection channel;
step S20, before sample analysis starts, pure gas is introduced into an analysis gas chamber of an element analysis instrument, when signals of a detection channel and a reference channel are stable, signal value average values of a period of time are taken as base lines respectively, the base line value of the detection channel is marked as BC0, and the base line value of the reference channel is marked as BR0;
step S30, after the sample begins to analyze, dividing each reference channel value RS [ i ] by a reference channel base line value BR0 to obtain a change coefficient KS [ i ], and dividing a detection channel base line value BC0 by the change coefficient KS [ i ] to obtain a real-time detection channel base line value BKS [ i ];
step S40, subtracting the real-time detection channel baseline value BKS [ i ] from the real-time read detection channel value CS [ i ] as a real-time signal integral value CI [ i ];
And S50, after the analysis of the sample is finished, accumulating the value obtained by looking up the linear table of each real-time signal integral value CI [ i ], and dividing the value by the weight of the sample to obtain the element content value in the sample.
A gas detection apparatus as a second aspect of the present invention for realizing a detection signal processing method of the above-described elemental analysis instrument, includes:
an analysis chamber having a gas input and a gas output;
The infrared light source is arranged at one side of the analysis air chamber and used for carrying out infrared irradiation on the gas to be detected in the analysis air chamber;
a detection channel infrared sensor disposed at the other side of the analysis gas chamber for detecting a gas concentration in the analysis gas chamber; and
The detection signal processing unit is connected with the detection channel infrared sensor and is used for processing detection signals; it is characterized in that the method comprises the steps of,
The infrared sensor is arranged on the other side of the analysis air chamber and connected with the detection signal processing unit, and is used for detecting the gas concentration in the analysis air chamber.
In a preferred embodiment of the present invention, a detection channel filter is provided between the analysis chamber and the detection channel infrared sensor.
In a preferred embodiment of the present invention, a reference channel filter is provided between the analysis chamber and the reference channel infrared sensor.
Due to the adoption of the technical scheme, the invention has the beneficial effects that: the invention adds a reference channel (the sampling frequency is synchronous with the detection channel) on the basis of the existing single detection channel, because the reference channel uses the same infrared light source, the same optical channel and the same detection channel as the detection channel, all physical states are consistent with the detection channel to serve as the physical basis of dynamic compensation, the detection signal wave band of the reference channel is the wave band which is never appeared in the sample gas and the carrier gas, and is generally 3.9 mu, the change of the detection channel directly reflects the change of the signal caused by the change of the temperature, the pressure and the flow velocity in the sample analysis process, and the baseline of the detection channel is dynamically corrected in real time through the change, so that the baseline of the detection channel is consistent with the change of the actual signal, and the consistency of the baseline and the fluctuation is ensured. According to the invention, in the sample analysis process, errors of analysis results caused by baseline fluctuation due to the existence of atmospheric pressure, ambient temperature and detected gas temperature impact on the infrared detection component and the change of the infrared detection component (such as drift of an infrared light source and change of a light absorption coefficient caused by pollution of an infrared light path) in the use environment are dynamically compensated, so that the detection precision is greatly improved, the correction times of an instrument are reduced, and the rapid detection performance of the instrument is improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of a conventional gas detection device for elemental analysis.
Fig. 2 is a schematic diagram of the structure of the gas detection device of the present invention.
Detailed Description
The invention is further described with reference to the following detailed drawings in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the implementation of the invention easy to understand.
The invention relates to a detection signal processing method of an elemental analysis instrument, which comprises the following steps:
step S10, adding a reference channel on the basis of a detection channel of an element analysis instrument, wherein the sampling frequency of the reference channel is synchronous with the sampling frequency of the detection channel;
step S20, before sample analysis starts, pure gas is introduced into an analysis gas chamber of an element analysis instrument, when signals of a detection channel and a reference channel are stable, signal value average values of a period of time are taken as base lines respectively, the base line value of the detection channel is marked as BC0, and the base line value of the reference channel is marked as BR0;
step S30, after the sample begins to analyze, dividing each reference channel value RS [ i ] by a reference channel base line value BR0 to obtain a change coefficient KS [ i ], and dividing a detection channel base line value BC0 by the change coefficient KS [ i ] to obtain a real-time detection channel base line value BKS [ i ];
step S40, subtracting the real-time detection channel baseline value BKS [ i ] from the real-time read detection channel value CS [ i ] as a real-time signal integral value CI [ i ];
And S50, after the analysis of the sample is finished, accumulating the value obtained by looking up the linear table of each real-time signal integral value CI [ i ], and dividing the value by the weight of the sample to obtain the element content value in the sample.
The invention adds a reference channel (the sampling frequency is synchronous with the detection channel) on the basis of the existing single detection channel, because the reference channel uses the same infrared light source, the same optical channel and the same detection channel as the detection channel, all physical states are consistent with the detection channel to serve as the physical basis of dynamic compensation, the detection signal wave band of the reference channel is the wave band which is never appeared in the sample gas and the carrier gas, and is generally 3.9 mu, the change of the detection channel directly reflects the change of the signal caused by the change of the temperature, the pressure and the flow velocity in the sample analysis process, and the baseline of the detection channel is dynamically corrected in real time through the change, so that the baseline of the detection channel is consistent with the change of the actual signal, and the consistency of the baseline and the fluctuation is ensured. According to the invention, errors of analysis results caused by baseline fluctuation due to the existence of atmospheric pressure, ambient temperature and detected gas temperature impact on the infrared detection component and the change of the infrared detection component (such as drift of an infrared light source and change of a light absorption coefficient caused by pollution of an infrared light path) in the sample analysis process are dynamically compensated, so that the detection precision is greatly improved.
The infrared detection air chamber in the traditional mode and the infrared detection air chamber in the reference mode are simultaneously installed on the same element analysis instrument, so that the environment where the two analysis air chambers are located and the pressure and the temperature of the gas introduced into the air chambers are consistent. Nine days of continuous testing, 6 samples were analyzed each time, and the average daily value was counted as follows. The long-term stability of the reference pattern of the present invention is significantly better than the conventional pattern.
| Time of | Reference mode at 35 DEG C | Conventional mode at 35 DEG C | Atmospheric pressure (hPa) |
| First day | 1.33973 | 1.337366154 | 1022.7 |
| The next day | 1.33813 | 1.340826014 | 1019.8 |
| Third day | 1.34668 | 1.270047692 | 1019.7 |
| Fourth day | 1.33682 | 1.306636643 | 1017.7 |
| Fifth day | 1.31987 | 1.32986979 | 1031.6 |
| Sixth day | 1.33716 | 1.32281986 | 1026.7 |
| Seventh day | 1.330295 | 1.36511014 | 1034.7 |
| Eighth day | 1.3254 | 1.329441958 | 1027.1 |
| Ninth day of | 1.32924 | 1.372355385 | 1020.3 |
| Average value of | 1.333702778 | 1.330497071 | |
| Relative standard deviation | 0.006147706 | 0.022840363 | |
| Standard deviation of | 0.008199212 | 0.030389036 |
Even if the outlier of traditional pattern 1.27 was removed the third day, the long-term stability advantage of the reference pattern was still very evident, with the following statistics:
Referring to fig. 2, there is shown a gas detection apparatus of the present invention, which implements the detection signal processing method of the above-mentioned elemental analysis instrument, including an analysis gas cell 100, an infrared light source 200, a detection channel infrared sensor 300, a reference channel infrared sensor 400, a detection channel filter 500, a reference channel filter 600, and a detection signal processing unit (not shown in the drawing).
The analysis chamber 100 has a gas input 110 and a gas output 120, which are in communication with the external atmosphere, respectively. The sample to be tested enters the combustion furnace, meanwhile, raw gas is input, the sample to be tested is heated and oxidized in the combustion furnace to become relevant gaseous substances, such as carbon or oxygen element becomes CO 2, released CO 2 enters the analysis air chamber 100 through the gas input end 110 under the driving of the raw gas, and after the detection is finished, the sample is discharged through the gas output end 120.
The infrared light source 200 is disposed at one side of the analysis gas chamber 100, and is used for infrared irradiation of the gas to be detected in the analysis gas chamber 100.
The detection channel infrared sensor 300 is provided at the other side of the analysis gas chamber 100, and is used to detect the concentration of gas within the analysis gas chamber 100.
The reference channel infrared sensor 400 is disposed at the other side of the analysis gas chamber 100 and is arranged in parallel with the detection channel infrared sensor 300 for detecting the concentration of the gas within the analysis gas chamber 100.
The detection channel filter 500 is disposed between the analysis chamber 100 and the detection channel infrared sensor 300.
The reference channel filter 600 is disposed between the analysis chamber 100 and the reference channel infrared sensor 400.
The detection signal processing unit is connected with the detection channel infrared sensor 300 and the reference channel infrared sensor 400 respectively, and is used for acquiring detection signals acquired by the detection channel infrared sensor 300 and the reference channel infrared sensor 400 in real time and processing the acquired detection signals in real time.
The light intensity I 0 of the infrared light emitted by the infrared light source 200, the light intensity I 1 reduced after the detected gas is absorbed by the detection channel infrared sensor 300, and then the extinction degree I 1/I0 reflects the concentration of the detected gas. The reduced light intensity I 2 of the reference channel infrared sensor 400 after receiving the detected gas is not affected by the concentration of the detected gas. Because the detected gas does not react in the wave band of the reference channel, the extinction degree I 2/I0 only reflects the physical quantity change state including the infrared light source and the analysis air chamber, and can be used for compensating the drift of the whole detection device.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A detection signal processing method of an elemental analysis instrument, comprising the steps of:
step S10, adding a reference channel on the basis of a detection channel of an element analysis instrument, wherein the sampling frequency of the reference channel is synchronous with the sampling frequency of the detection channel;
step S20, before sample analysis starts, pure gas is introduced into an analysis gas chamber of an element analysis instrument, when signals of a detection channel and a reference channel are stable, signal value average values of a period of time are taken as base lines respectively, the base line value of the detection channel is marked as BC0, and the base line value of the reference channel is marked as BR0;
step S30, after the sample begins to analyze, dividing each reference channel value RS [ i ] by a reference channel base line value BR0 to obtain a change coefficient KS [ i ], and dividing a detection channel base line value BC0 by the change coefficient KS [ i ] to obtain a real-time detection channel base line value BKS [ i ];
step S40, subtracting the real-time detection channel baseline value BKS [ i ] from the real-time read detection channel value CS [ i ] as a real-time signal integral value CI [ i ];
And S50, after the analysis of the sample is finished, accumulating the value obtained by looking up the linear table of each real-time signal integral value CI [ i ], and dividing the value by the weight of the sample to obtain the element content value in the sample.
2. A gas detection apparatus for realizing the detection signal processing method of the elemental analysis meter according to claim 1, comprising:
an analysis chamber having a gas input and a gas output;
The infrared light source is arranged at one side of the analysis air chamber and used for carrying out infrared irradiation on the gas to be detected in the analysis air chamber;
a detection channel infrared sensor disposed at the other side of the analysis gas chamber for detecting a gas concentration in the analysis gas chamber; and
The detection signal processing unit is connected with the detection channel infrared sensor and is used for processing detection signals; it is characterized in that the method comprises the steps of,
The infrared sensor is arranged on the other side of the analysis air chamber and connected with the detection signal processing unit, and is used for detecting the gas concentration in the analysis air chamber.
3. The gas detection apparatus according to claim 2, wherein a detection channel filter is provided between the analysis chamber and the detection channel infrared sensor.
4. The gas detection apparatus according to claim 2, wherein a reference channel filter is provided between the analysis chamber and the reference channel infrared sensor.
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| CN102809546A (en) * | 2012-08-21 | 2012-12-05 | 南京埃森环境技术有限公司 | Low-concentration flue gas infra-red analyzer and detection method |
| CN104713841A (en) * | 2015-02-09 | 2015-06-17 | 中国石油大学(华东) | Self-calibration analyzer design method and device |
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| CN107036994A (en) * | 2017-05-25 | 2017-08-11 | 北京雪迪龙科技股份有限公司 | A kind of non-dispersion infrared gas analyzer of dynamic reference and the method for detecting gas concentration |
| CN209589768U (en) * | 2019-02-19 | 2019-11-05 | 河南郑大零醛屋环保科技有限公司 | A kind of indoor gas detection analysis instrument |
| CN214066918U (en) * | 2020-10-29 | 2021-08-27 | 湖北锐意自控系统有限公司 | Ultraviolet gas analyzer |
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| CN102809546A (en) * | 2012-08-21 | 2012-12-05 | 南京埃森环境技术有限公司 | Low-concentration flue gas infra-red analyzer and detection method |
| CN104713841A (en) * | 2015-02-09 | 2015-06-17 | 中国石油大学(华东) | Self-calibration analyzer design method and device |
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