CN101819194A - Standard sample dilution deviation tracking and correcting system calibrated by gas analyzer on line and method thereof - Google Patents
Standard sample dilution deviation tracking and correcting system calibrated by gas analyzer on line and method thereof Download PDFInfo
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Abstract
The invention discloses a specimen dilution deviation tracking and correcting system calibrated by a gas analyzer on line and a method thereof. The specimen dilution tracking deviation correcting system comprises a master control computer, a calibrated gas analyzer and a calibration instrument, wherein the calibrated gas analyzer is communicated with a gas circuit of the calibration instrument via a diluted specimen delivery valve; the calibration instrument is communicated with gas circuits of a zero gas generator and a standard air storage vessel for dilution; the master control computer is respectively connected with the calibrated gas analyzer, the diluted specimen delivery valve, the calibration instrument and the zero air generator electrically; the calibrated gas analyzer is communicated with a gas circuit of a dilution-free standard air storage vessel via a dilution-free specimen delivery valve; and the dilution-free specimen delivery valve is electrically connected with the master control computer. The invention overcomes the deficiency of the traditional gas analyzer in on-line calibration technology, can find out the defective condition of the calibration instruction performance, and obtains the best effect of reducing the standard sample concentration error by a simple and practical technological method; and the working procedure is simple and facilitates the control of the master control computer.
Description
Technical field
The present invention relates to test and analysis technology and analytical instrument flow process integrated technology, a kind of standard sample dilution deviation tracking and correcting system and method for gas analysis instrument on-line calibration is provided especially.
Background technology
In order to tackle, solve the problem of environmental pollution that is caused because of contemporary industry production and human settlements life style, people need carry out continuously the concentration of the gas pollutant of various tool harmfulness in the surrounding air, accurately, monitoring widely; Thereby set up and spread all over the world enormous amount, system complex environment air automatic monitor station point.And relying on modern test and analysis technology development level, this class automatic monitor station point is constructed at specific gas pollutant project, is integrated in unmanned machine room, special-purpose automatic test assay laboratory.The main body of its workflow is the gas analysis instrument of various on-line operations, provides concentration data about tested gaseous contamination substrate concentration continuously by them.
Gas analysis instrument can provide the concentration data of tested gas componant, be to utilize this tested gas componant under controlled physics, electrochemical conditions effect, certain physical quantity signal of distinctive optics, electricity, thermodynamics, dynamics and so on can be produced, and the objective phenomenon and the rule of quantitative equation can be set up between this signal span numerical value and the tested gas concentration numerical value.Thereby carry out the gas analysis instrument calibration, and be exactly to carry the standard model (abbreviation standard specimen) of the tested gas of concentration known to it, and, adjust used quantitative equation according to instrument response concentration and standard specimen concentration, make both reach consistent.
Yet the gas analysis instrument of modern technologies manufacturing is monitored in the application automatically at the environmental air pollution thing of reality, also has following characteristics:
(1) make tested gas produce required physical quantity signal, analytical instrument sensing physics, electrochemical conditions partly, or because of carrying gaseous sample thermodynamics, dynamics index different times difference by a relatively large margin, or the fouling products that brings because of sample adheres to, the influence of retention degree, or be etched process rotten, fatigue deformation slowly because of contact material, or the like, all may make existing quantitative equation no longer suitable, cause the data error that surpasses specified limit, thereby need carry out on-line calibration regular, routine to gas analysis instrument with standard specimen.
(2) monitoring of environmental air pollution substrate concentration belongs to the test analysis of micro substance more, gas analysis instrument need use the high Weak Physical Quantity signal detection device of sensitivity (photomultiplier for example, high-resolution is infrared, the ultraviolet light photo sensor, accurate temperature-sensitive, thermal conductivity detector (TCD) or the like).And this type of high sensitivity detector spare that modern technologies are made, for quite slight self material aging, change in quality, stain with structure displacement, distortion also very sensitive.In its Acceptable life scope, the variation of randomness can take place in the detection sensitivity that shows, make existing quantitative equation no longer suitable, cause the data error that surpasses specified limit, thereby need carry out on-line calibration regular, routine to gas analysis instrument with standard specimen.
(3) at the website scene, be used for the special component of on-line calibration gas analysis instrument span, the standard specimen of specific concentrations, be by the standard specimen dosing apparatus that is called as calibration instrument, zero gas (being all extremely low gas of content of the material of measurand and loss measurand) with target flow, conflux and mix with the standard gas (gas that promptly contains the high concentration measurand) of target flow, dynamic dilution produces the standard specimen of required composition, desired concn; And carry by relevant water conservancy diversion device and connecting tube.Owing to be the test analysis of trace level, the concentration that span is calibrated required standard specimen is very low, the undesirable condition that occurred by aspects such as sealing, cleanliness, unobstructed property influences easily, and makes the standard specimen concentration substantial deviation calibration instrument calculating of actual acquisition, the result of regulation and control.This need to differentiate, to take precautions against undesirable condition effectively, be avoided misapplying the incorrect standard specimen of actual concentrations and carry out the gas analysis instrument calibration by analytical instrument on-line calibration operation regular, routine.
As seen, quality index (as accuracy, uncertainty etc.) for the data that gas analysis instrument provides of controlling continuous on-line operation, can continue to remain within the scope that is subordinate to the requirement of data quality management system, just must be at website machine room scene, for each analysis project provides the standard specimen dispenser, to carry out the regular on-line calibration of gas analysis instrument automatically.The typical structure diagrammatic sketch of this standard specimen dispenser as shown in Figure 1.Among the figure:
1, the dilution of required composition is with standard gas high pressure storage steel bottle (being furnished with the output reduction valve).
2, Zero gas generator, usually and other analysis projects shared.
3, calibration instrument, usually and other analysis projects shared.
4, dilution standard specimen transfer valve.
5, be calibrated gas analysis instrument.
6, main control computer (or acting on identical device), usually and other analysis projects shared.
Among the figure, dotted line is represented computer control circuit, and solid line is represented the sample gas circuit.
Its principle of work and flow process are: main control computer 6 is according to subscribing the activity duration layout, when being calibrated gas analysis instrument 5 and calibrating, standard specimen transfer valve 4 is open-minded, with required standard specimen preparation index and parameter (for example standard specimen composition, standard specimen concentration, standard airshed, zero airshed etc.) input calibration instrument 3; Make calibration instrument 3 get the standard gas of target flow, appointment composition and concentration from standard gas high pressure storage steel bottle 1, and get the zero gas of target flow from Zero gas generator 2, confluxing to mix produces the dynamic dilution standard specimen, immerses through standard specimen transfer valve 4 to be calibrated gas analysis instrument 5; Standard specimen concentration is calculated by following formula:
Standard specimen concentration=dilution is with standard gas concentration * dilution gfactor, wherein:
Continue to carry the standard specimen time enough, be calibrated gas analysis instrument 5 response concentration readings stable after; If this response concentration and standard specimen concentration differ above specified scope, then main control computer 6 regulation and control are calibrated gas analysis instrument 5 and quote new quantitative equation, make response concentration reach consistent with standard specimen concentration, otherwise continue to use original quantitative equation; After finishing, standard specimen transfer valve 4 cuts out, and calibration instrument 5 stops to prepare standard specimen.
Around here, the gas analysis instrument on-line calibration that provides with above-mentioned dynamic dilution technology is according to the numerical relation result calculated of dilution with standard gas concentration, standard airshed and zero airshed with the concentration of standard specimen.And standard airshed and zero airshed are to be measured and regulated by flowmeter in the calibration instrument and control device thereof; The error in dipping of the used flowmeter of calibration instrument can directly cause the standard specimen concentration error.This brings risk obviously for enforcement analytical instrument on-line calibration and causes the technology limitation to improving data quality level.
In real work, more rigorous data quality management system can require regularly (for example per season) to website machine room scene, with the flowmeter of working stamndard, the used flowmeter of calibration instrument is tested and is calibrated.Nonetheless, before carrying out this operation,, will cause incorrect standard specimen to be misapplied next time, make the ability that gas analysis instrument loses thus provides correct data that is calibrated if the error in dipping of the used flowmeter of calibration instrument has exceeded acceptability limit; These incorrect data can not be differentiated and be rejected worse, and directly arrive the data user.
For quality control index can be implemented in real work, the data quality management system can only leave enough loose acceptability limit for the error in dipping of the used flowmeter of calibration instrument, promptly reduces data accuracy (or uncertainty) controlling index.
The defective that above-mentioned standard specimen dispenser exists aspect the flow metering error has limited the operation of gas analysis instrument on-line calibration and can't obtain the more data of pin-point accuracy.We should research and design can real-time judge calibration instrument flow metering error degree, and can subdue or compensate the technical method of standard specimen concentration error effectively; Implement more to optimize, reliably, gas analysis instrument on-line calibration accurately.
Above-mentioned standard specimen density calculating method shows, the error in dipping of calibration instrument standard airshed and zero airshed departs from the dilution deviation of result of calculation by causing dilution, and linearity is delivered in the standard specimen concentration.If can quantitatively calculate dilution deviation, can judge the calibration instrument performance condition, and can revise standard specimen concentration thus; By reducing the standard specimen concentration error, improve the correctness and the precision of calibration result.
Summary of the invention
At above-mentioned defective of the prior art, the object of the present invention is to provide a kind of standard sample dilution deviation tracking and correcting system and method for improved gas analysis instrument on-line calibration.
The technical solution adopted in the present invention: a kind of standard sample dilution deviation tracking and correcting system of gas analysis instrument on-line calibration, comprise main control computer, be calibrated gas analysis instrument and calibration instrument, the described gas analysis instrument that is calibrated is communicated with the gas circuit of calibration instrument by dilution standard specimen transfer valve, described calibration instrument and Zero gas generator, dilution are communicated with the gas circuit of standard gas storage container, described main control computer respectively be calibrated gas analysis instrument, dilute the standard specimen transfer valve, calibration instrument, Zero gas generator be electrically connected; The described gas analysis instrument that is calibrated also is communicated with the gas circuit of exempting from dilution standard gas storage container by exempting to dilute the standard specimen transfer valve, describedly exempts to dilute the standard specimen transfer valve and main control computer is electrically connected.
Above-mentioned dilution is to dilute with standard gas high pressure storage steel bottle with standard gas storage container.
The above-mentioned dilution standard gas storage container of exempting from is for exempting from dilution standard gas high pressure storage steel bottle.
The above-mentioned gas that is calibrated that is calibrated in the gas analysis instrument (5) is CO, or SO
2, or NO.
The present invention provides a kind of standard sample dilution deviation tracking modification method of the gas analysis instrument on-line calibration based on above-mentioned standard sample dilution deviation tracking and correcting system simultaneously, may further comprise the steps:
(a) it is open-minded to exempt to dilute the standard specimen transfer valve, make the standard gas of exempting from the dilution standard gas storage container enter and be calibrated gas analysis instrument through exempting to dilute the standard specimen transfer valve, it is enough to wait to continue the transfer criteria gas time, is calibrated reading after the gas analysis instrument response concentration stabilize, and calculates response coefficient;
(b) close behind the completing steps (a) and exempt to dilute the standard specimen transfer valve;
(c) it is open-minded to dilute the standard specimen transfer valve, with required standard specimen preparation index and parameter input calibration instrument, make calibration instrument from diluting with the standard gas of getting target flow, appointment composition and concentration the standard gas storage container, and from Zero gas generator, get the zero gas of target flow, conflux and mix the standard specimen that produces dynamic dilution, enter through dilution standard specimen transfer valve then and be calibrated gas analysis instrument, it is enough to wait to continue to carry the standard specimen time, be calibrated reading after the gas analysis instrument response concentration stabilize, and calculate dilution deviation;
(d), calculate the standard specimen concentration that finally is used to be calibrated the gas analysis instrument calibration according to the dilution deviation of above-mentioned acquisition.
Response coefficient in the above-mentioned steps (a) is calculated as follows:
Dilution deviation in the above-mentioned steps (c) is calculated as follows:
Wherein:
Standard specimen concentration in the above-mentioned steps (d) is calculated as follows:
Standard specimen concentration=(dilution) * dilution deviation with standard gas concentration * dilution gfactor
The present invention has overcome defective and the deficiency that traditional gas analysis instrument on-line calibration technology exists, and can in time find calibration instrument performance undesirable condition, can obtain to reduce the best effects of standard specimen concentration error with the most simple and practical technical method.Need in website is integrated, not increase new varieties equipment and equipment---in fact just need a valve and one bottle of standard gas of using, work flow is simple, is convenient to the control of main control computer more.
Description of drawings
Fig. 1 is the typical structure synoptic diagram of traditional standard specimen dispenser;
Fig. 2 is the structural representation of standard specimen dispenser of the present invention;
Fig. 3 is the specific embodiment structural representation of standard specimen dispenser of the present invention.
Embodiment
Below in conjunction with accompanying drawing concrete structure of the present invention is further described.
In the present invention, carry out the quantitative measuring and calculating of dilution deviation, be the standard gas that utilizes analysis project with good degree of stability and accuracy---CO standard gas for example, by directly carrying near the standard gas (exempt from dilute standard specimen) of calibration with standard specimen concentration to this project analysis instrument, and carry the spike effect of the calibration of calibration instrument dynamic dilution preparation with generation between the standard specimen (dilution standard specimen), calculate calibration instrument near used standard airshed and zero airshed, the dilution deviation that has.
On the principle, the dilution deviation of calibration instrument only reflects the influence of standard airshed and zero airshed error in dipping, and the standard specimen because of the preparation heterogeneity does not change.So on integrated morphology, only need to select the standard specimen dispenser that is used to produce spike effect Analysis project, change into as Fig. 2 and get final product.Wherein:
1, the dilution of required composition is with standard gas high pressure storage steel bottle (being furnished with the output reduction valve).
2, Zero gas generator, usually and other analysis projects shared.
3, calibration instrument, usually and other analysis projects shared.
4, dilution standard specimen transfer valve.
5, be calibrated gas analysis instrument.
6, main control computer (or acting on identical device), usually and other analysis projects shared.
7, required composition exempts from dilution (concentration near calibration use standard specimen) standard gas high pressure storage steel bottle (being furnished with the output reduction valve).
8, exempt to dilute the standard specimen transfer valve.
Among the figure, dotted line is represented computer control circuit, and solid line is represented the sample gas circuit.
As shown in Figure 2, the standard sample dilution deviation tracking and correcting system of gas analysis instrument on-line calibration of the present invention, comprise main control computer 6, be calibrated gas analysis instrument 5 and calibration instrument 3, the described gas analysis instrument 5 that is calibrated is communicated with the gas circuit of calibration instrument 3 by dilution standard specimen transfer valve 4, described calibration instrument 3 and Zero gas generator 2, dilution is communicated with the gas circuit of standard gas storage container 1 (dilution with standard gas high pressure storage steel bottle), described main control computer 6 respectively be calibrated gas analysis instrument 5, dilution standard specimen transfer valve 4, calibration instrument 3, Zero gas generator 2 is electrically connected; The described gas analysis instrument 5 that is calibrated also is communicated with the gas circuit of exempting from dilution standard gas storage container 7 (exempting from dilution standard gas high pressure storage steel bottle) by exempting to dilute standard specimen transfer valve 8, describedly exempts to dilute standard specimen transfer valve 8 and is electrically connected with main control computer 6.
The principle of work and the flow process of above-mentioned standard sample dilution deviation tracking and correcting system are as follows, and main control computer 6 is according to subscribing the activity duration layout, when being calibrated gas analysis instrument 5 and calibrating:
(a) it is open-minded to exempt to dilute standard specimen transfer valve 8, makes standard gas in the standard gas high pressure storage steel bottle 7, enters and is calibrated analytical instrument 5 through exempting to dilute the standard specimen transfer valve; It is enough to continue the transfer criteria gas time, is calibrated reading after the gas analysis instrument 5 response concentration stabilize; Be calculated as follows response coefficient:
(b) close after finishing and exempt to dilute standard specimen transfer valve 8.
(c) standard specimen transfer valve 4 is open-minded, with required standard specimen preparation index and parameter (for example standard specimen composition, standard specimen concentration, standard airshed, zero airshed etc.) input calibration instrument 3; Make calibration instrument 3 get the standard gas of target flow, appointment composition and concentration from standard gas high pressure storage steel bottle 1, and get the zero gas of target flow from Zero gas generator 2, conflux and mix the standard specimen that produces dynamic dilution, enter through standard specimen transfer valve 4 and be calibrated gas analysis instrument 5; Continue to carry the standard specimen time enough, be calibrated reading after the gas analysis instrument 5 response concentration stabilize; Be calculated as follows dilution deviation:
Wherein:
(d) be calculated as follows the standard specimen concentration that finally is used for the analytical instrument calibration:
Standard specimen concentration=(dilution) * dilution deviation with standard gas concentration * dilution gfactor
If be calibrated the response concentration and the standard specimen concentration of analytical instrument 5 and differ above specified scope this moment, then main control computer 6 regulation and control are calibrated gas analysis instrument 5 and quote new quantitative equation, make response concentration reach consistent, otherwise continue to use original quantitative equation with standard specimen concentration; After finishing, standard specimen transfer valve 4 cuts out, and calibration instrument 5 stops to prepare standard specimen.
The dilution deviation that obtains thus calculates the standard specimen concentration of the analysis project of other shared these calibration instruments, and is effectively same---as long as standard airshed and zero airshed can be close when calculating this dilution deviation.Thereby the standard specimen dispenser of other analysis projects of shared this calibration instrument, still as shown in Figure 1.But its principle of work and flow process change in the present invention:
Standard specimen concentration=(dilution) * dilution deviation with standard gas concentration * dilution gfactor
Wherein:
If be calibrated the response concentration and the standard specimen concentration of analytical instrument 5 and differ above specified scope this moment, then main control computer 6 regulation and control are calibrated gas analysis instrument 5 and quote new quantitative equation, make response concentration reach consistent, otherwise continue to use original quantitative equation with standard specimen concentration; After finishing, standard specimen transfer valve 4 cuts out, and calibration instrument 5 stops to prepare standard specimen.
In addition, dilution deviation also has the effect that quantizes to differentiate calibration instrument 3 performances.In real work, can conclude mutatis mutandis numerical range to it as required.If surpass mutatis mutandis numerical range, then calibration instrument 3 off-lines keeped in repair.
Be illustrated in figure 3 as a specific embodiment of the present invention---the structural representation of air supervisory system, among the figure, dotted line is represented computer control circuit, and solid line is represented the sample gas circuit, the selected spike effect Analysis project CO that produces.Configuration CO exempts from dilution standard gas concentration 18 μ mol/mol, adopts and mixes steel cylinder standard gas, and wherein, configuration CO dilutes with standard gas concentration 4000 μ mol/mol; Configuration SO
2Dilution is with standard gas concentration 100 μ mol/mol; Configuration NO dilutes with standard gas concentration 100 μ mol/mol.Calibration instrument is with standard airshed 32ml/min (target), and zero airshed 8500ml/min (target) prepares the calibration standard specimen.Adopt standard sample dilution deviation tracking modification method mentioned above can calculate the standard specimen concentration that obtains to be used for the analytical instrument calibration apace, thereby realize the on-line calibration of gas analysis instrument, it is simple to have work flow, is convenient to the characteristics such as control of main control computer.
Claims (8)
1. the standard sample dilution deviation tracking and correcting system of a gas analysis instrument on-line calibration, comprise main control computer (6), be calibrated gas analysis instrument (5) and calibration instrument (3), the described gas analysis instrument (5) that is calibrated is communicated with the gas circuit of calibration instrument (3) by dilution standard specimen transfer valve (4), described calibration instrument (3) and Zero gas generator (2), dilution is communicated with the gas circuit of standard gas storage container (1), described main control computer (6) respectively be calibrated gas analysis instrument (5), dilution standard specimen transfer valve (4), calibration instrument (3), Zero gas generator (2) is electrically connected; It is characterized in that, also comprise and exempt from dilution standard gas storage container (7), this is exempted from dilution standard gas storage container and is communicated with the gas circuit that is calibrated gas analysis instrument (5) by exempting to dilute standard specimen transfer valve (8), describedly exempts to dilute standard specimen transfer valve (8) and is electrically connected with main control computer (6).
2. according to the standard sample dilution deviation tracking and correcting system of the described gas analysis instrument on-line calibration of claim 1, it is characterized in that described dilution is to dilute with standard gas high pressure storage steel bottle with standard gas storage container (1).
3. according to the standard sample dilution deviation tracking and correcting system of the described gas analysis instrument on-line calibration of claim 1, it is characterized in that the described dilution standard gas storage container (7) of exempting from is for exempting from dilution standard gas high pressure storage steel bottle.
4. according to the standard sample dilution deviation tracking and correcting system of the described gas analysis instrument on-line calibration of claim 1, it is characterized in that the described gas that is calibrated that is calibrated in the gas analysis instrument (5) is CO, or SO
2, or NO.
5. the standard sample dilution deviation tracking modification method based on the gas analysis instrument on-line calibration of the described standard sample dilution deviation tracking and correcting system of claim 1 is characterized in that, may further comprise the steps:
(a) it is open-minded to exempt to dilute standard specimen transfer valve (8), make the standard gas of exempting from the dilution standard gas storage container (7) enter and be calibrated gas analysis instrument (5) through exempting to dilute the standard specimen transfer valve, it is enough to wait to continue the transfer criteria gas time, be calibrated reading after gas analysis instrument (5) the response concentration stabilize, and calculate response coefficient;
(b) close behind the completing steps (a) and exempt to dilute standard specimen transfer valve (8);
(c) it is open-minded to dilute standard specimen transfer valve (4), with required standard specimen preparation index and parameter input calibration instrument (3), make calibration instrument (3) from diluting with getting target flow the standard gas storage container (1), specify the standard gas of composition and concentration, and from Zero gas generator (2), get the zero gas of target flow, conflux and mix the standard specimen that produces dynamic dilution, enter through dilution standard specimen transfer valve (4) then and be calibrated gas analysis instrument (5), it is enough to wait to continue to carry the standard specimen time, be calibrated reading after gas analysis instrument (5) the response concentration stabilize, and calculate dilution deviation;
(d), calculate the standard specimen concentration that finally is used to be calibrated gas analysis instrument (5) calibration according to the dilution deviation of above-mentioned acquisition.
6. according to the standard sample dilution deviation tracking modification method of the described gas analysis instrument on-line calibration of claim 5, it is characterized in that the response coefficient in the described step (a) is calculated as follows:
7. according to the standard sample dilution deviation tracking modification method of the described gas analysis instrument on-line calibration of claim 5, it is characterized in that the dilution deviation in the described step (c) is calculated as follows:
Wherein:
8. according to the standard sample dilution deviation tracking modification method of the described gas analysis instrument on-line calibration of claim 5, it is characterized in that the standard specimen concentration in the described step (d) is calculated as follows:
Standard specimen concentration=(dilution) * dilution deviation with standard gas concentration * dilution gfactor.
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| CN102749423A (en) * | 2012-07-26 | 2012-10-24 | 嘉兴长天环保科技有限公司 | Intelligent environment online monitoring and automatically-comparing quality control instrument |
| CN103226098A (en) * | 2013-01-10 | 2013-07-31 | 中国航空工业集团公司西安飞机设计研究所 | Method for accuracy calibration of airplane extinguishant concentration test system |
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| CN105974062A (en) * | 2016-06-03 | 2016-09-28 | 中国矿业大学 | Gas sensor calibration device and calibration method thereof |
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| CN102749423A (en) * | 2012-07-26 | 2012-10-24 | 嘉兴长天环保科技有限公司 | Intelligent environment online monitoring and automatically-comparing quality control instrument |
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| CN103226098A (en) * | 2013-01-10 | 2013-07-31 | 中国航空工业集团公司西安飞机设计研究所 | Method for accuracy calibration of airplane extinguishant concentration test system |
| CN104090067A (en) * | 2013-08-12 | 2014-10-08 | 力合科技（湖南）股份有限公司 | Gas continuous-monitoring system realizing automatic standard gas inspection |
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| CN111693409A (en) * | 2020-05-27 | 2020-09-22 | 北京蛙鸣华清环保科技有限公司 | Gas and biological aerosol calibration system and method |
| CN111693409B (en) * | 2020-05-27 | 2023-08-15 | 北京蛙鸣华清环保科技有限公司 | Gas and biological aerosol calibration system and method |
| CN111735870A (en) * | 2020-07-31 | 2020-10-02 | 暨南大学 | Correction method and correction device for online real-time analysis of mass spectrum |
| CN111999375A (en) * | 2020-09-30 | 2020-11-27 | 暨南大学 | Exhaled volatile organic compound quantification method based on real-time online mass spectrometry |
| CN113588883A (en) * | 2021-08-02 | 2021-11-02 | 中科三清科技有限公司 | Ambient air quality monitoring device for automatic calibration |
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