CN104267198A - Automatic calibration device and method for volatile organic compound analyzer - Google Patents
Automatic calibration device and method for volatile organic compound analyzer Download PDFInfo
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- CN104267198A CN104267198A CN201410349987.8A CN201410349987A CN104267198A CN 104267198 A CN104267198 A CN 104267198A CN 201410349987 A CN201410349987 A CN 201410349987A CN 104267198 A CN104267198 A CN 104267198A
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Abstract
The invention relates to an automatic calibration device and method mainly applied in the environmental monitoring field, and specifically relates to an automatic calibration device and method for volatile organic compound analysis. The device comprises a six-way valve, a multi-position valve having a common inlet and a common outlet, a plurality of quantitative loops with increasing volumes in sequence, a rotor flowmeter and a carrier-gas bottle. Therefore, the automatic calibration device has the following advantages that (1) operations are convenient and automatic calibration for the volatile organic compound analyzer can be realized; (2) the device has a simple structure and relatively low production and maintenance cost; and (3) calibration cost is saved, relatively low standard gas consumption is required for calibration; and cost is relatively low.
Description
Technical field
The present invention relates to a kind of automatic calibration equipment and method, be mainly used in environmental monitoring field, be specifically related to a kind of automatic calibration equipment for volatile organic matter analysis and method.
Background technology
In environmental sample, organic compound is usually by vapor-phase chromatography or Qi Xiang Se Pu – analytical reagent composition.Organic compound can produce electric signal in the detecting device of chromatogram or Se Pu – mass spectrometer, the size of electric signal is directly proportional to the concentration (or quality) of organic compound, therefore can measure by the concentration (or quality) of the electric signal size detected to organic compound in sample.But, due to chromatogram or Se Pu – mass spectrum, the detection to organic compound is indirect detection, electric signal that same concentrations (or quality) organic compound of different nature produces in same chromatogram or Se Pu – mass spectrum is different, the same organic compound of same concentrations (or quality) under the different operating condition of same chromatogram or Se Pu – mass spectrometer and the electric signal that produces of different chromatogram or Se Pu – mass spectrometer not identical yet.Therefore, need to analyze with standard model, determine the concentration (or quality) of each organic compound under a certain analysis condition of analyser and the linear dependence of electric signal, draw the response curve of each organic compound concentrations to electric signal, quantitative for each organic compound.This process is called as the demarcation (or correction) to analyser.
In gas, volatile organic compounds (VOCs) on-line continuous monitoring usual Xi attached Nong Suo – thermal desorption chromatogram or Chromatography/Mass Spectrometry method measure, existing demarcation (or correction) method mainly contains two kinds: one uses dynamic dilution instrument, series concentration calibrating gas being diluted to needs directly enters analytic system analysis, and this method wastes expensive calibrating gas very much; Another kind method is formulated in sample can needing the calibrating gas of concentration with dynamic dilution instrument, then sample can is connected on analyser analyzes, and this method needs dynamic dilution instrument, clear tank instrument and sample can, and expense is expensive equally, complicated operation.
Therefore, lower and automatic calibration equipment and the method for calibrating gas can be saved in the urgent need to developing a kind of cost for volatile organic matter analysis.
Summary of the invention
The present invention mainly solves technical matterss such as " Apparatus and method for cost are higher " and " the useless calibrating gas of wave " existing for prior art, provides a kind of automatic calibration equipment for volatile organic matter analysis and method.Adopt the automatic Calibration that this Apparatus and method for can realize volatile organic matter analyser, this calibration facility structure is simple, and this scaling method is easy to operate, and uses this Apparatus and method for institute quota of expenditure gas less, and expense is lower.
Above-mentioned technical matters of the present invention is mainly solved by following technical proposals:
For an automatic calibration equipment for volatile organic matter analyser, comprising: six-way valve, several quantitative loop, spinner-type flowmeter, the carrier gas bottle that increase successively with the multi-position valve of public inlet end and public endpiece, volume, wherein:
6 valve position of described six-way valve are linked in sequence the public inlet end of the calibrating gas bottle of gas to be measured, spinner-type flowmeter, the public endpiece of multi-position valve, volatile organic matter analyser injection port, carrier gas bottle, multi-position valve successively;
Described in described multi-position valve increases successively with volume respectively, several quantitative loop are connected.
Optimize, above-mentioned a kind of automatic calibration equipment for volatile organic matter analyser, described multi-position valve is ten two-position valves, described ten two-position valves comprise: public circulation gas circuit C and public circulation gas circuit D, described public circulation gas circuit C is provided with a public inlet end A and 6 low level port, described circulation gas circuit D is provided with a public endpiece B and 6 high-order port, the ingress port of described quantitative loop is connected with described low level port respectively, and the outlet port of described quantitative loop is connected with described high-order port respectively.
Optimize, above-mentioned a kind of automatic calibration equipment for volatile organic matter analyser, described quantitative loop is 6, each inlet end of described quantitative loop is connected to 6 low level ports successively clockwise according to the order that the volume of affiliated quantitative loop is ascending, each endpiece of described quantitative loop is connected to 6 high-order ports successively clockwise according to the order that the volume of affiliated quantitative loop is ascending
Utilize automatic calibration equipment described in claim 1 to carry out a method of demarcating, comprising:
Step 401, to be sent into calibrating gas by the switching of six-way valve and ten two-position valves after in several quantitative loop again by spinner-type flowmeter emptying;
Step 402, carrier gas to be sent in step 401 quantitative loop used by the automatic switchover of six-way valve, 12 valves and produce mixed gas after mixing with the calibrating gas in this quantitative loop, again described mixed gas is sent into volatile organic matter analyser, the response signal of recorder analyser;
Step 403, enters the concentration of the mixed gas of analyser according to the volume computing of carrier gas used in the volume of the concentration of calibrating gas used in step 401 and quantitative loop, step 402;
Step 404, the concentration signal pair comprising described response signal information and described mixed gas concentration is built, according to described concentration signal to the correlativity for building described response signal and described mixed gas concentration according to the described mixed gas concentration in the described response signal in step 402 and step 403;
Step 405, repeats the operation of step 401-404 to next quantitative loop, until obtain concentration signal pair corresponding to all quantitative loop;
Step 406, responds and concentration standard curve preparation according to multiple concentration signals that step 405 obtains.
Optimize, the above-mentioned automatic calibration equipment that utilizes carries out the method for demarcating, and the flow direction of the calibrating gas in described step 401 is followed successively by: public inlet end A, the circulation gas circuit C of No. 1 position of six-way valve, No. 6 positions of six-way valve, ten two-position valves, quantitative loop, circulation gas circuit D, the public endpiece B of ten two-position valves, No. 3 positions of six-way valve, No. 2 positions of six-way valve, spinner-type flowmeter.
Optimize, the above-mentioned automatic calibration equipment that utilizes carries out the method for demarcating, and the carrier gas in described step 402 flows to and is followed successively by: No. 5 positions of six-way valve, No. 6 positions of six-way valve, the public inlet end A of ten two-position valves, circulation gas circuit C, quantitative loop; Mixed gas in described step 402 flows to and is followed successively by: the public endpiece B of quantitative loop, circulation gas circuit D, ten two-position valves, No. 3 positions of six-way valve, No. 4 positions of six-way valve, volatile organic matter analyser injection port.
Optimize, the above-mentioned automatic calibration equipment that utilizes carries out the method for demarcating, and the described response signal in described step 402 is the peak heights of the peak area of the chromatographic peak of electric signal or the chromatographic peak of electric signal.
Optimize, the above-mentioned automatic calibration equipment that utilizes carries out the method for demarcating, and the response in described step 406 and the preparation of concentration standard curve are by by the mixed gas concentration of multiple concentration signal centering and response signal information, described point in two-dimensional coordinate system obtains.
Therefore, tool of the present invention has the following advantages: 1. easy to operate, can realize the automatic Calibration to volatile organic matter analyser; 2. device structure is simple, produce and maintenance cost lower; 3. save calibration cost, demarcate the calibrating gas consumed less, expense is lower.
Accompanying drawing explanation
Fig. 1 is the structural drawing of the automatic calibration equipment of the embodiment of the present invention.
Fig. 2 is the automatic calibration method gas sampling flow process of the embodiment of the present invention.
Fig. 3 is automatic calibration method gas sampling and the analysis process of the embodiment of the present invention.
Embodiment
Below by embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.
Embodiment:
As shown in Figure 1, a kind of automatic calibration equipment for volatile organic matter analyser, comprise: six-way valve, several quantitative loop, spinner-type flowmeter, the carrier gas bottle that increase successively with the multi-position valve of public inlet end and public endpiece, volume, wherein: 6 valve position of six-way valve connect the public inlet end of the calibrating gas bottle of gas to be measured, spinner-type flowmeter, the public endpiece of multi-position valve, volatile organic matter analyser injection port, carrier gas bottle, multi-position valve successively; The valve position of multi-position valve from low to high order is provided with the described quantitative loop that volume increases successively.
Multi-position valve is ten two-position valves in the present embodiment, and quantitative loop is 6.Ten two-position valves comprise: public circulation gas circuit C and public circulation gas circuit D, the low level port one, low level port 2, low level port 3, low level port 4, low level port 5, the low level port 6 that public circulation gas circuit C are provided with public inlet end A and set gradually by clock-wise order, accordingly, at high-order port 7, high-order port 8, high-order port 9, high-order port 10, high-order port 11, high-order port 12 that circulation gas circuit D is provided with public endpiece B and sets gradually by clock-wise order.The inlet end of 6 quantitative loop is connected on low level port 1-6 according to the order that the volume of affiliated quantitative loop is ascending successively, and each endpiece of quantitative loop is connected to high-order port 7-12 successively according to the order that the volume of affiliated quantitative loop is ascending.
As shown in Figure 2, adopt after said structure, the automatic calibration equipment calibrating gas method of sampling of the present embodiment and flow process are: sent into by six-way valve and ten two-position valves successively by calibrating gas after in several quantitative loop again by spinner-type flowmeter emptying; For quantitative loop 1, calibrating gas is by six-way valve port one and 6, the public inlet end A entered on the circulation gas circuit C of ten two-position valves enters circulation gas circuit C, then quantitative loop 1 is entered from the port one circulation gas circuit C, enter public endpiece B from this quantitative loop outlet port 7 entered circulation gas circuit D again, and then flow out from public outlet B, enter six-way valve port 3 and 2 by pipeline, finally enter flowmeter emptying, complete calibrating gas quantitative loop sampling routine.Quantitative loop 2 is identical with quantitative loop 1 to the sampling routine of quantitative loop 6.
As shown in Figure 3, after adopting said structure, the automatic calibration equipment gas sampling analytical approach of the present embodiment and flow process are: carrier gas to be sent in step 401 quantitative loop used by six-way valve and ten two-position valves and produce mixed gas after mixing with the calibrating gas in this quantitative loop, again described mixed gas is sent into volatile organic matter analyser, the response signal of recorder analyser; For quantitative loop 1, carrier gas is by six-way valve port 5 and 6, enter the public inlet end A on 12 valve circulation gas circuit C, enter quantitative loop entrance 1, calibrating gas in quantitative loop is purged the port 7 entered on circulation gas circuit D, then enter six-way valve port 3 and 4 by circulation gas circuit D from public outlet B, finally enter analyser and carry out analysis demarcation; Step 402 is the automatic switchovers by six-way valve, 12 valves, quantitatively to be purged by the calibrating gas in quantitative loop enter analytic system with carrier gas, carries out analysis and measures, for demarcate analysis system, complete calibrating gas sample introduction and routine analyzer.Quantitative loop 2 is identical with quantitative loop 1 to the injection procedure of quantitative loop 6.
By the conversion of different size quantitative loop, the calibrating gas of same concentration different volumes can be joined in analyser and analyze, reach the object of demarcation (correction) analyser.Calibrating gas sampling and the operation of purging sample introduction are completed automatically by software control.
After sampling and sample introduction, need the conversion carrying out automatic Calibration instrument standard gas concentration.For the calibrating gas of the 1ppm concentration of 1ml, if enter analyser with 500m carrier gas purge, being equivalent to 500ml concentration is that the calibrating gas of 2.00ppb enters analyser; Add the calibrating gas of 1ppm concentration by 0.5ml, 2ml, 5ml and 10ml quantitative loop, enter analyser with 500ml carrier gas purge, be equivalent to the calibrating gas that 500ml concentration is respectively 1.00ppb, 4.00ppb, 10.00ppb and 20ppb and enter analyser.
After conversion, the preparation of automatic Calibration instrument typical curve can be carried out, 1ppm concentration standard gas is added respectively by 0.5ml, 1.0ml, 2.0ml, 5.0ml and 10.0ml quantitative loop, enter analyser with 500ml carrier gas purge, be equivalent to the calibrating gas that 500ml concentration is respectively 1.00ppb, 4.00ppb, 10.00ppb and 20ppb and enter analyser; According to the typical curve of the concentration preparation response after the response signal (peak area or peak height) of analyser and corresponding conversion with concentration.
Wherein, response can by by response signal information and corresponding converted score, described point in two-dimensional coordinate system obtains to the typical curve of concentration.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (8)
1. for an automatic calibration equipment for volatile organic matter analyser, it is characterized in that, comprising: six-way valve, several quantitative loop, spinner-type flowmeter, the carrier gas bottle that increase successively with the multi-position valve of public inlet end and public endpiece, volume, wherein:
6 valve position of described six-way valve are linked in sequence the public inlet end of the calibrating gas bottle of gas to be measured, spinner-type flowmeter, the public endpiece of multi-position valve, volatile organic matter analyser injection port, carrier gas bottle, multi-position valve successively;
Described in described multi-position valve increases successively with volume respectively, several quantitative loop are connected.
2. a kind of automatic calibration equipment for volatile organic matter analyser according to claim 1, it is characterized in that, described multi-position valve is ten two-position valves, described ten two-position valves comprise: public circulation gas circuit C and public circulation gas circuit D, described public circulation gas circuit C is provided with a public inlet end A and 6 low level port, described circulation gas circuit D is provided with a public endpiece B and 6 high-order port, the ingress port of described quantitative loop is connected with described low level port respectively, and the outlet port of described quantitative loop is connected with described high-order port respectively.
3. a kind of automatic calibration equipment for volatile organic matter analyser according to claim 2, it is characterized in that, described quantitative loop is 6, each inlet end of described quantitative loop is connected to 6 low level ports successively clockwise according to the order that the volume of affiliated quantitative loop is ascending, and each endpiece of described quantitative loop is connected to 6 high-order ports successively clockwise according to the order that the volume of affiliated quantitative loop is ascending.
4. utilize automatic calibration equipment described in claim 1 to carry out a method of demarcating, it is characterized in that, comprising:
Step 401, to be sent into calibrating gas by the switching of six-way valve and ten two-position valves after in several quantitative loop again by spinner-type flowmeter emptying;
Step 402, carrier gas to be sent in step 401 quantitative loop used by the automatic switchover of six-way valve, 12 valves and produce mixed gas after mixing with the calibrating gas in this quantitative loop, again described mixed gas is sent into volatile organic matter analyser, the response signal of recorder analyser;
Step 403, enters the concentration of the mixed gas of analyser according to the volume computing of carrier gas used in the volume of the concentration of calibrating gas used in step 401 and quantitative loop, step 402;
Step 404, the concentration signal pair comprising described response signal information and described mixed gas concentration is built, according to described concentration signal to the correlativity for building described response signal and described mixed gas concentration according to the described mixed gas concentration in the described response signal in step 402 and step 403;
Step 405, repeats the operation of step 401-404 to next quantitative loop, until obtain concentration signal pair corresponding to all quantitative loop;
Step 406, responds and concentration standard curve preparation according to multiple concentration signals that step 405 obtains.
5. according to utilizing the automatic calibration equipment that utilizes described in claim 4 to carry out the method for demarcating, it is characterized in that, the flow direction of the calibrating gas in described step 401 is followed successively by: public inlet end A, the circulation gas circuit C of No. 1 position of six-way valve, No. 6 positions of six-way valve, ten two-position valves, quantitative loop, circulation gas circuit D, the public endpiece B of ten two-position valves, No. 3 positions of six-way valve, No. 2 positions of six-way valve, spinner-type flowmeter.
6. according to utilizing the automatic calibration equipment that utilizes described in claim 4 to carry out the method for demarcating, it is characterized in that, the carrier gas in described step 402 flows to and is followed successively by: No. 5 positions of six-way valve, No. 6 positions of six-way valve, the public inlet end A of ten two-position valves, circulation gas circuit C, quantitative loop; Mixed gas in described step 402 flows to and is followed successively by: the public endpiece B of quantitative loop, circulation gas circuit D, ten two-position valves, No. 3 positions of six-way valve, No. 4 positions of six-way valve, volatile organic matter analyser injection port.
7., according to utilizing the automatic calibration equipment that utilizes described in claim 4 to carry out the method for demarcating, it is characterized in that, the described response signal in described step 402 is the peak heights of the peak area of the chromatographic peak of electric signal or the chromatographic peak of electric signal.
8. according to utilizing the automatic calibration equipment that utilizes described in claim 4 to carry out the method for demarcating, it is characterized in that, the response in described step 406 and the preparation of concentration standard curve are by by the mixed gas concentration of multiple concentration signal centering and response signal information, described point in two-dimensional coordinate system obtains.
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| CN201410349987.8A CN104267198B (en) | 2014-07-22 | 2014-07-22 | A kind of automatic calibration equipment for volatile organic matter analyzer and method |
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| CN201410349987.8A CN104267198B (en) | 2014-07-22 | 2014-07-22 | A kind of automatic calibration equipment for volatile organic matter analyzer and method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104597154A (en) * | 2015-01-08 | 2015-05-06 | 聚光科技(杭州)股份有限公司 | Device and method for detecting VOC (volatile organic compound) in liquid |
| CN106645522A (en) * | 2016-08-31 | 2017-05-10 | 武汉市天虹仪表有限责任公司 | On-line volatile organic compound monitoring system with automatic calibration function |
| CN107490644A (en) * | 2017-09-25 | 2017-12-19 | 北京鹏宇昌亚环保科技有限公司 | A kind of automatic calibration device and gas chromatograph |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104597154A (en) * | 2015-01-08 | 2015-05-06 | 聚光科技(杭州)股份有限公司 | Device and method for detecting VOC (volatile organic compound) in liquid |
| CN106645522A (en) * | 2016-08-31 | 2017-05-10 | 武汉市天虹仪表有限责任公司 | On-line volatile organic compound monitoring system with automatic calibration function |
| CN107490644A (en) * | 2017-09-25 | 2017-12-19 | 北京鹏宇昌亚环保科技有限公司 | A kind of automatic calibration device and gas chromatograph |
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