CN104267198B - A kind of automatic calibration equipment for volatile organic matter analyzer and method - Google Patents
A kind of automatic calibration equipment for volatile organic matter analyzer and method Download PDFInfo
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- CN104267198B CN104267198B CN201410349987.8A CN201410349987A CN104267198B CN 104267198 B CN104267198 B CN 104267198B CN 201410349987 A CN201410349987 A CN 201410349987A CN 104267198 B CN104267198 B CN 104267198B
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Abstract
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 and method of analyzing for volatile organic matter. Wherein equipment comprises: comprising: six-way valve, with the multiposition valve of public arrival end and the public port of export, several quantitative rings, spinner flowmeter, the carrier gas bottle that volume increases successively. Therefore, tool of the present invention has the following advantages: 1. and easy to operate, can realize the automatic Calibration to volatile organic matter analyzer; 2. device structure is simple, and production and maintenance cost are lower; 3. save calibration cost, demarcate the calibrating gas consuming less, expense is lower.
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 and method of analyzing for volatile organic matter.
Background technology
In environmental sample, organic compound is conventionally by gas chromatography or Qi Xiang Se Pu – analytical reagent composition. Organic compound can produce the signal of telecommunication in the detector of chromatogram or Se Pu – mass spectrometer, the size of the signal of telecommunication is directly proportional to the concentration of organic compound (or quality), therefore can the concentration (or quality) to organic compound in sample measure by the signal of telecommunication size detecting. But, because chromatogram or Se Pu – mass spectrum are indirect detection to the detection of organic compound, the signal of telecommunication difference that same concentrations (or quality) organic compound of different nature produces in same chromatogram or Se Pu – mass spectrum, the same organic compound of same concentrations (or quality) under the different operating condition of same chromatogram or Se Pu – mass spectrometer and the signal of telecommunication that produces of different chromatogram or Se Pu – mass spectrometer not identical yet. Therefore, need to analyze with standard sample, determine the concentration (or quality) of each organic compound under a certain analysis condition of analyzer and the linear dependence of the signal of telecommunication, draw the response curve of each organic compound substrate concentration to the signal of telecommunication, for to each organic compound quantitatively. This process is called as the demarcation (or correction) to analyzer.
The monitoring of VOC in gas (VOCs) on-line continuous is measured by the attached Nong Suo of Xi – thermal desorption chromatogram or Chromatography/Mass Spectrometry method conventionally, existing demarcation (or correction) method mainly contains two kinds: one is to use dynamic dilution instrument, calibrating gas is diluted to the series concentration needing and directly enters analytical system analysis, this method is wasted expensive calibrating gas very much; Another kind method is to need the calibrating gas of concentration to be formulated in sample can with dynamic dilution instrument handle, then sample can is connected on analyzer and is analyzed, and this method needs dynamic dilution instrument, clear tank instrument and sample can, and expense is expensive equally, complicated operation.
Therefore, in the urgent need to developing a kind of automatic calibration equipment and the method that cost for volatile organic matter analysis is lower and can save calibrating gas.
Summary of the invention
The present invention solves the technical problem such as prior art existing " Apparatus and method for cost is higher " and " the useless calibrating gas of wave ", and a kind of automatic calibration equipment and method of analyzing for volatile organic matter is provided. Adopt this Apparatus and method for can realize the automatic Calibration to volatile organic matter analyzer, this calibration facility is simple in structure, 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 problem of the present invention is mainly solved by following technical proposals:
For an automatic calibration equipment for volatile organic matter analyzer, comprising: six-way valve, with the multiposition valve of public arrival end and the public port of export, several quantitative rings, spinner flowmeter, the carrier gas bottle that volume increases successively, wherein:
Be linked in sequence the successively public port of export, volatile organic matter analyzer injection port, carrier gas bottle, the public arrival end of multiposition valve of calibrating gas bottle, spinner flowmeter, multiposition valve of gas to be measured of 6 valve position of described six-way valve;
Described several that described multiposition valve increases successively with volume respectively quantitatively encircle and are connected.
Optimize, above-mentioned a kind of automatic calibration equipment for volatile organic matter analyzer, described multiposition 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 public arrival end A and 6 low level ports, described circulation gas circuit D is provided with public port of export B and 6 high-order ports, the ingress port of described quantitative ring is connected with described low level port respectively, and the outlet port of described quantitative ring is connected with described high-order port respectively.
Optimize, above-mentioned a kind of automatic calibration equipment for volatile organic matter analyzer, described quantitative ring is 6, each arrival end of described quantitative ring is connected in 6 low level ports successively clockwise according to the ascending order of the volume of affiliated quantitative ring, each port of export of described quantitative ring is connected in 6 high-order ports successively clockwise according to the ascending order of the volume of affiliated quantitative ring
Utilize the method that automatic calibration equipment is demarcated described in claim 1, comprising:
Step 401, the switching by six-way valve and ten two-position valves by calibrating gas send into several quantitatively after in ring again by spinner flowmeter emptying;
Step 402, automatic switchover by six-way valve, 12 valves is sent into carrier gas in step 401 quantitative ring used and with the calibrating gas in this quantitatively encircles and is mixed the rear mist that produces, again described mist is sent into volatile organic matter analyzer, the response signal of recorder analyser;
Step 403, adds the concentration into the mist of analyzer according to the stereometer of carrier gas used in the volume of the concentration of calibrating gas used in step 401 and quantitative ring, step 402;
Step 404, build the concentration signal pair that comprises described response signal information and described mixed gas concentration according to the described mixed gas concentration in the described response signal in step 402 and step 403, according to described concentration signal to the correlation for building described response signal and described mixed gas concentration;
Step 405, quantitatively encircles and repeats the operation of step 401-404 the next one, until obtain concentration signal pair corresponding to all quantitative rings;
Step 406, the multiple concentration signals that obtain according to step 405 are to preparation response and concentration standard curve.
Optimize, the above-mentioned method of utilizing automatic calibration equipment to demarcate, the flow direction of the calibrating gas in described step 401 is followed successively by: public arrival 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 ring, circulation gas circuit D, the public port of export B of ten two-position valves, No. 3 positions of six-way valve, No. 2 positions of six-way valve, spinner flowmeter.
Optimize, the above-mentioned method of utilizing automatic calibration equipment to demarcate, carrier gas in described step 402 flows to and is followed successively by: public arrival end A, the circulation gas circuit C of No. 5 positions of six-way valve, No. 6 positions of six-way valve, ten two-position valves, quantitative ring; Mist in described step 402 flows to and is followed successively by: quantitatively ring, circulation gas circuit D, the public port of export B of ten two-position valves, No. 3 positions of six-way valve, No. 4 positions of six-way valve, volatile organic matter analyzer injection port.
Optimize the above-mentioned method of utilizing automatic calibration equipment to demarcate, the peak area of chromatographic peak that the described response signal in described step 402 is the signal of telecommunication or the peak heights of the chromatographic peak of the signal of telecommunication.
Optimize, the above-mentioned method of utilizing automatic calibration equipment to demarcate, the response in described step 406 and the preparation of concentration standard curve are by by the mixed gas concentration of multiple concentration signal centerings and response signal information, described point in two-dimensional coordinate system obtains.
Therefore, tool of the present invention has the following advantages: 1. and easy to operate, can realize the automatic Calibration to volatile organic matter analyzer; 2. device structure is simple, and production and maintenance cost are lower; 3. save calibration cost, demarcate the calibrating gas consuming less, expense is lower.
Brief description of the drawings
Fig. 1 is the structure chart 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.
Detailed description of the invention
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 analyzer, comprise: six-way valve, with the multiposition valve of public arrival end and the public port of export, several quantitative rings, spinner flowmeter, the carrier gas bottle that volume increases successively, wherein: 6 valve position of six-way valve connect the public port of export, volatile organic matter analyzer injection port, the carrier gas bottle of calibrating gas bottle, spinner flowmeter, the multiposition valve of gas to be measured, the public arrival end of multiposition valve successively; The valve position of multiposition valve from low to high order is provided with the described quantitative ring that volume increases successively.
Multiposition valve is ten two-position valves in the present embodiment, and quantitatively ring is 6. Ten two-position valves comprise: public circulation gas circuit C and public circulation gas circuit D, on public circulation gas circuit C, be provided with public arrival end A and the low level port one setting gradually by clockwise order, low level port 2, low level port 3, low level port 4, low level port 5, low level port 6, accordingly, be provided with public port of export B and the high-order port 7 setting gradually by clockwise order, high-order port 8, high-order port 9, high-order port 10, high-order port 11, high-order port 12 at circulation gas circuit D. 6 arrival ends that quantitatively encircle are connected in low level port 1-6 above successively according to the ascending order of the volume of affiliated quantitative ring, and quantitatively each port of export of ring is connected in high-order port 7-12 successively according to the ascending order of the volume of affiliated quantitative ring.
As shown in Figure 2, adopt after said structure, the automatic calibration equipment calibrating gas method of sampling and the flow process of the present embodiment are: after calibrating gas is sent into in several quantitative rings by six-way valve and ten two-position valves successively, pass through spinner flowmeter emptying again; Quantitatively to encircle 1 as example, calibrating gas is by six-way valve port one and 6, the public arrival end A entering on the circulation gas circuit C of ten two-position valves enters circulation gas circuit C, then the port one from circulation gas circuit C enters quantitative ring 1, enter public port of export B from this port 7 that quantitatively ring outlet enters 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 and quantitatively encircle sampling routine. Quantitative ring 2 is identical with quantitative ring 1 to the sampling routines that quantitatively encircle 6.
As shown in Figure 3, adopt after said structure, automatic calibration equipment gas sampling analytical method and the flow process of the present embodiment are: carrier gas is sent in step 401 quantitative ring used and with the calibrating gas in this quantitatively encircles and mixed the rear mist that produces by six-way valve and ten two-position valves, again described mist is sent into volatile organic matter analyzer, the response signal of recorder analyser; Quantitatively to encircle 1 as example, carrier gas is by six-way valve port 5 and 6, enter the public arrival end A on 12 valve circulation gas circuit C, enter quantitative ring entrance 1, calibrating gas in quantitatively encircling is purged to the port 7 entering 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 analyzer and analyze demarcation; Step 402 is by the automatic switchover of six-way valve, 12 valves, the calibrating gas in quantitative ring is quantitatively purged and enters analytical system with carrier gas, analyzes mensuration, for demarcating analytical system, completes calibrating gas sample introduction and routine analyzer. Quantitative ring 2 is identical with quantitative ring 1 to the sample introduction programs of quantitatively encircling 6.
By the quantitatively conversion of ring of different size, the calibrating gas of same concentration different volumes can be joined in analyzer and analyzes, reach the object of demarcation (correction) analyzer. Calibrating gas sampling and the operation of purging sample introduction are completed automatically by software control.
After sampling and sample introduction, need to carry out the conversion of automatic Calibration instrument calibrating gas concentration. Taking the calibrating gas of the 1ppm concentration of 1ml as example, if purge and enter analyzer with 500m carrier gas, the calibrating gas that is equivalent to 500ml concentration and is 2.00ppb enters analyzer; With 0.5ml, 2ml, 5ml and 10ml quantitatively ring add the calibrating gas of 1ppm concentration, enter analyzer with 500ml carrier gas purging, be equivalent to the calibrating gas that 500ml concentration is respectively 1.00ppb, 4.00ppb, 10.00ppb and 20ppb and enter analyzer.
After converting, can carry out the preparation of automatic Calibration instrument calibration curve, add respectively 1ppm concentration standard gas with the quantitative ring of 0.5ml, 1.0ml, 2.0ml, 5.0ml and 10.0ml, purge and enter analyzer with 500ml carrier gas, be equivalent to the calibrating gas that 500ml concentration is respectively 1.00ppb, 4.00ppb, 10.00ppb and 20ppb and enter analyzer; Calibration curve according to the concentration preparation response after the response signal of analyzer (peak area or peak height) and corresponding conversion with concentration.
Wherein, response can be by by response signal information and corresponding conversion concentration, described point in two-dimensional coordinate system obtains with the calibration 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 amendments or supplement or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Claims (5)
1. a method of utilizing automatic calibration equipment to demarcate, is characterized in that, uses based on oneIn the automatic calibration equipment of volatile organic matter analyzer, comprising: six-way valve, with public arrival endWith the multiposition valve of the public port of export, several quantitative rings, spinner flowmeter that volume increases successively, carryGas cylinder, wherein:
6 valve position of described six-way valve be linked in sequence successively calibrating gas bottle, the rotor flow of gas to be measuredMeter, the public port of export of multiposition valve, volatile organic matter analyzer injection port, carrier gas bottle, multiposition valvePublic arrival end;
Described several that described multiposition valve increases successively with volume respectively quantitatively encircle and are connected;
Described multiposition valve is ten two-position valves, and described ten two-position valves comprise: public circulation gas circuit C and publicCirculation gas circuit D, described public circulation gas circuit C is provided with public arrival end A and 6 low level ports, instituteState circulation gas circuit D and be provided with public port of export B and 6 high-order ports, the arrival end of described quantitative ringMouthful be connected with described low level port respectively, the outlet port of described quantitative ring respectively with described high-order portBe connected;
Described quantitative ring is 6, and each arrival end of described quantitative ring is according to the volume of affiliated quantitative ringAscending order is connected in 6 low level ports successively clockwise, each outlet of described quantitative ringEnd is connected in 6 high-order ports successively clockwise according to the ascending order of the volume of affiliated quantitative ring,
The method that this automatic calibration equipment is demarcated specifically comprises:
Step 101, sends calibrating gas into several by the switching of six-way valve and ten two-position valves and quantitatively encirclesIn one after again by spinner flowmeter emptying;
Step 102, sends carrier gas into step 101 by the automatic switchover of six-way valve, 12 valves usedAfter quantitatively mixing in ring and with the calibrating gas in this quantitative ring, produce mist, then by described mixingGas is sent into volatile organic matter analyzer, the response signal of recorder analyser;
Step 103, according to volume, the step of the concentration of calibrating gas used in step 101 and quantitative ringIn 102, the stereometer of carrier gas used is added the concentration into the mist of analyzer;
Step 104, according to the described gaseous mixture in described response signal and step 103 in step 102Bulk concentration builds the concentration signal pair that comprises described response signal information and described mixed gas concentration, rootAccording to described concentration signal to the correlation for building described response signal and described mixed gas concentration;
Step 105, quantitatively encircles to the next one operation that repeats step 101-104, until obtain instituteThere is the concentration signal pair that quantitative ring is corresponding;
Step 106, the multiple concentration signals that obtain according to step 105 are to preparation response and concentration standard songLine.
2. the method for utilizing automatic calibration equipment to demarcate according to claim 1, its featureBe, the flow direction of the calibrating gas in described step 101 is followed successively by: No. 1 position, six of six-way valve leads toNo. 6 positions of valve, the public arrival end A of ten two-position valves, circulation gas circuit C, quantitatively ring, circulation gas circuit D,The public port of export B of ten two-position valves, No. 3 positions of six-way valve, No. 2 positions of six-way valve, spinner flowmeter.
3. the method for utilizing automatic calibration equipment to demarcate according to claim 2, its featureBe, carrier gas in described step 102 flows to and is followed successively by: 6 of No. 5 positions of six-way valve, six-way valvePublic arrival end A, the circulation gas circuit C of number position, ten two-position valves, quantitative ring; In described step 102Mist flows to and is followed successively by: the quantitatively public port of export B, six of ring, circulation gas circuit D, ten two-position valvesNo. 3 positions, No. 4 positions of six-way valve, the volatile organic matter analyzer injection port of logical valve.
4. the method for utilizing automatic calibration equipment to demarcate according to claim 3, its featureBe peak area or the telecommunications of the chromatographic peak that the described response signal in described step 102 is the signal of telecommunicationNumber the peak heights of chromatographic peak.
5. the method for utilizing automatic calibration equipment to demarcate according to claim 4, its featureBe, the response in described step 106 and the preparation of concentration standard curve are by multiple concentration is believedMixed gas concentration and response signal information described point in two-dimensional coordinate system of number centering obtain.
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| CN104597154B (en) * | 2015-01-08 | 2016-08-31 | 聚光科技(杭州)股份有限公司 | In liquid, VOC detects device and method |
| 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 |
| CN107490644B (en) * | 2017-09-25 | 2020-12-08 | 北京鹏宇昌亚环保科技有限公司 | Be applied to gas chromatograph's automatic calibration device and gas chromatograph |
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| CN101329228B (en) * | 2008-07-29 | 2010-09-15 | 北京大学 | Peroxy acyl radical nitric acid lipid substance sampling system and detection method |
| CN203688432U (en) * | 2013-12-17 | 2014-07-02 | 中兴仪器（深圳）有限公司 | Liquid metering system |
| CN204008668U (en) * | 2014-07-22 | 2014-12-10 | 武汉市天虹仪表有限责任公司 | A kind of automatic calibration equipment for volatile organic matter analyser |
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