CN202041512U - Analysis device - Google Patents
Analysis device Download PDFInfo
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- CN202041512U CN202041512U CN2011200464648U CN201120046464U CN202041512U CN 202041512 U CN202041512 U CN 202041512U CN 2011200464648 U CN2011200464648 U CN 2011200464648U CN 201120046464 U CN201120046464 U CN 201120046464U CN 202041512 U CN202041512 U CN 202041512U
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- gas
- temperature
- permeate chamber
- sample
- osmos tube
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Abstract
The utility model relates to an analysis device, which comprises a seeping chamber unit, a flow rate control unit and at least one seeping pipe, wherein the seeping pipe is provided with a standard air source, gas volatilized from the seeping pipe is inner standard gas, the seeping chamber unit comprises a seeping chamber and a temperature measuring element, the seeping pipe is arranged in the seeping chamber, the seeping chamber is respectively connected with sample gas and a sample inlet module of an analysis instrument, and the flow rate control unit controls the flow rate of the sample gas. The analysis device has the advantages that the structure is simple, the cost is low, the service life is long, in addition, the inner standard gas concentration can be controlled, ingredients of the inner standard gas can be expanded according to requirements, and the like.
Description
Technical field
The utility model relates to a kind of analytical equipment, and it is mainly used in the quantified system analysis, especially in chromatogram, mass spectrum and the spectroscopic analysis system.
Background technology
In quantitative test, generally need to use internal standard method and external standard method (also being calibration curve method).
External standard method is a kind of by setting up the relation curve between sample response value and its concentration, the method for sample being carried out quantitative test.
In external standard method, because the chromatographic condition of each sample analysis is very difficult identical, as: analysis result appears than mistake in the response performance of detecting device, column temperature, mobile phase flow rate and composition, sample size etc. easily; And external standard method can't compensate the variation of component to be measured in the pre-treatment process, therefore generally seldom uses in the miniaturization instrument.
Internal standard method is a kind of by selecting the reference substance of suitable material as component to be measured, it quantitatively is added in the testing sample goes, the method that the amount that the ratio of foundation component to be measured and the response of reference substance on detecting device and reference substance add is carried out quantitative test.
Internal standard method has overcome in the external standard method, and when carrying out the testing sample analysis, chromatographic condition is difficult to identical and quantitative error that cause at every turn.Internal standard method joins reference substance in the testing sample and goes, component to be measured and reference substance are analyzed under same chromatographic condition, quantitative accuracy is improved, particularly how much irrelevant the ratio of the component to be measured of internal mark method determination and reference material response under same testing conditions and sample size be, and this can eliminate in the external standard method fully because the error of the inaccurate generation of sample size.
The variation of sample size, the subtle change of chromatographic condition are little to inner mark method ration result's influence, particularly testing sample are being carried out adding internal standard compound before the pre-treatment, and then are carrying out pre-treatment, can partly compensate the loss of component to be measured when sample pre-treatments.If obtain high-precision result, can add multiple internal standard compound, to improve the precision of quantitative test.The key of internal standard method is to select suitable internal standard compound, and the amount of internal standard compound component best and to be measured is close.
In the express-analysis instrument, generally standard specimen (interior gas) is stored in gas cylinder, during sample introduction at the scene, control by stream switching and solenoid valve, after sample gas to be analyzed and the standard specimen in the gas cylinder are mixed, enter the sample introduction module again, enter analytic system analysis then.What the Hapsite type portable gas chromatography of Inficon company-GC-MS adopted is exactly aforesaid way.This method has realized interior gas is added sample gas, has improved the quantitative test ability of instrument, but has had following shortcoming:
1, the gas cylinder finite volume of gas in the dress, gas only can use tens times in one bottle, needs often to change equipment operation expense height;
2, the amount that needs gas in the strict control, and interior gas need mix with sample gas, and the gas flow path design is complicated, causes the instruments design complexity, and is bulky, cost height, poor reliability;
3, the concentration change wide ranges of on-the-spot testing sample, and the interior gas concentration in the gas gas cylinder is unadjustable, the mark implementation makes the bad adaptability of on-the-spot testing sample in this kind;
4, same gas cylinder only can charge into the close limited several gases of physicochemical property, and much active chemistry can not use gas cylinder, and therefore interior gas kind is few;
5, bottled gas is because the interaction of the variation of pressure or gas cylinder inside surface and gas composition causes standard gas accuracy decline, thereby is not easy to be traceable to NIST, and EPA standard and ASTM standard are not approved.
The utility model content
In order to solve above-mentioned deficiency of the prior art, the analytical equipment that the utility model provides that a kind of apparatus structure is simple, cost is low, long service life and interior gas concentration may command, component can expand by demand.
For achieving the above object, the utility model adopts following technical scheme:
The utility model also provides a kind of analytical equipment, comprises permeate chamber unit, flow controlling unit and at least one osmos tube;
Described osmos tube is the gas source, and the gas that evaporates from osmos tube is interior gas;
Described permeate chamber unit comprises permeate chamber and temperature element; Described osmos tube is arranged in the permeate chamber; Described permeate chamber links to each other with the sample introduction module of sample gas and analytical instrument respectively;
The flow of described flow controlling unit control sample gas.
As preferably, described analytical equipment also comprises heating element and temperature conditioning unit, is used for the permeate chamber heating and regulates temperature in the permeate chamber.
Further, described temperature conditioning unit and/or flow controlling unit are integrated in the analytical instrument.
Further, described analytical instrument is chromatogram, mass spectrum or chromatograph-mass spectrometer coupling analyser.
As preferably, fill different chemical substances in the different osmos tubes, by changing or select gas kind in the osmos tube adjustment.
Above-mentioned analytical approach and device adopt osmos tube, and be based on: osmos tube is a miniaturization device of being made by porous film material, in the osmos tube the inside chemical substance are housed, and this chemical substance is in the biphase equilibrium state of gas phase and liquid phase (perhaps solid phase).
When osmos tube is under definite temperature, gaseous chemical substance can infiltrate from osmos tube with the permeability of determining.The gaseous chemical substance that infiltrates from osmos tube becomes the gas of concentration known by the carrier gas proportioning, the calibrating gas of using as quantitative test.The concentration of the calibrating gas that osmos tube produces is by the permeability of osmos tube and the flow decision of carrier gas; Sample gas is as carrier gas, and the sample airshed is controlled by flow control system; Gas permeability is only determined by the character and the residing permeate chamber temperature of osmos tube of chemical substance.This shows that gas concentration is by the gas kind, osmos tube temperature and carrier gas flux determine; After gas was determined, gas concentration only depended on osmos tube temperature and carrier gas flux.
In the gas generator of being made by osmos tube, the concentration of gas is by permeate chamber temperature and carrier gas flux decision.The computing formula of gas concentration is:
Wherein C is a gas volume concentration, the ppm of unit; P is a permeability, the ng/min of unit; Mw is a molecular weight gas; Fc is the total flow of gas combination gas, the cc/min of unit; 24.46 be the molar volume of gas under standard conditions; Km is the molecular weight constant.
When osmos tube is under definite temperature, gaseous compound can infiltrate from osmos tube with the permeability of determining.Permeability is as follows with the relation of temperature:
logP
1＝logP
0+α(T
1-T
0)
P wherein
0Be T
0Permeability under the temperature, P
1Be T
1Permeability under the temperature, α is a temperature coefficient.
Traditional air distributing device based on osmos tube need be equipped with independently temperature control system and flow control system, and is bulky, and complex structure can't be used for small-sized analytical instrument.
The utility model compared with prior art has following beneficial effect:
1, long service life
Different with common gas cylinder finite capacity, an osmos tube can use more than 1 year at least;
2, system architecture is compact simple, and volume is little, and is in light weight
Interior gas mixes with sample gas in permeate chamber, and only by the permeability decision of gas, flow path designs is simple for the amount of interior gas; Can directly be installed on sampling conduit or be integrated in hand-held probe inside;
Simultaneously, because the flow controlling unit of control criterion gas concentration and temperature conditioning unit all overlap with analytical instrument shared, make system architecture compact simple, volume is little, and is in light weight;
3, cost is low
The cost of osmos tube simultaneously, does not need complicated magnetic valve controller to come the amount of gas in the strict control far below bottled gas, and cost reduces significantly;
4, interior gas concentration may command
By the flow of change sample gas or the temperature in the residing permeate chamber of osmos tube, the concentration of gas in can in very wide scope, changing;
5, interior gas kind is convenient adjusts
Only need simply remove or increase the kind that osmos tube just can increase and decrease interior gas easily;
6, concentration precision height
Can be traceable to NIST, EPA standard and ASTM standard are all approved the gas generating means based on osmos tube.
Description of drawings
Fig. 1 is the structural representation of analytical equipment among the embodiment 1;
Fig. 2 is the structural representation of analytical equipment among the embodiment 2;
Fig. 3 is the structural representation of analytical equipment among the embodiment 3;
Fig. 4 be among the embodiment 3 in the graph of relation of gas permeability and temperature.
Embodiment
Embodiment 1
See also Fig. 1, a kind of analytical equipment comprises permeate chamber unit, temperature conditioning unit 31, flow controlling unit 41 and osmos tube 11;
Described osmos tube 11 is for being filled with the Dynacal type osmos tube of pure bromine phenyl-pentafluoride, and osmos tube length is 1cm, and diameter is 6.35mm; Described osmos tube 11 is the gas source, and the bromine phenyl-pentafluoride gas that evaporates from osmos tube 11 is interior gas;
Described permeate chamber unit comprises permeate chamber 21, heating element and temperature element; Described heating element and temperature element are arranged on the inside of permeate chamber 21, do not mark in the drawings; Described permeate chamber 21 links to each other with the sample introduction module of sample gas and analytical instrument respectively, and sample gas is gas air to be analyzed in the utility model;
Described osmos tube 11 is arranged in the permeate chamber 21; Sample gas enters permeate chamber 21, and the calibrating gas that sample gas and interior gas form feeds the sample introduction module of analytical instrument;
Heating element heats permeate chamber 21, and temperature element is measured the temperature in the permeate chamber 21 in real time and fed back to the temperature conditioning unit 31 that is arranged on analytical instrument inside; Temperature conditioning unit 31 remains on needed temperature according to the heating of the actual temperature control heating element that records to permeate chamber 21 to guarantee the temperature in the permeate chamber 21, and then osmos tube 11 evaporates with certain permeability under design temperature; In the present embodiment, the temperature that permeate chamber 21 is set is 40 ℃;
Flow controlling unit 41 is arranged in the analytical instrument, and the flow of sample gas is controlled.
Present embodiment also provides a kind of analytical approach, may further comprise the steps:
A, provide present embodiment described analytical equipment;
B, the temperature that permeate chamber 21 is set are 40 ℃, and heating element heats permeate chamber 21, and temperature element is measured the temperature in the permeate chamber 21 in real time, and it is fed back to temperature conditioning unit 31, make the temperature in the permeate chamber 21 remain on 40 ℃; Under 40 ℃ temperature, the gas that is arranged in the osmos tube 11 in the permeate chamber 21 evaporates with certain permeability, and permeability is 12.6ng/min;
The flow of flow controlling unit 41 control sample gas is 20ml/min;
Sample gas feeds permeate chamber 21, will take out of from the interior gas that osmos tube 11 evaporates, and forms calibrating gas; In temperature is that 40 ℃, flow are under the condition of 20ml/min, in the calibrating gas in the concentration of gas be 50ppb;
C, calibrating gas feed the sample introduction module of analytical instrument, are used for quantitative test.
Embodiment 2
See also Fig. 2, a kind of analytical equipment, different with embodiment 1 described analytical equipment is: a plurality of osmos tubes are installed, to produce different interior gases in the permeate chamber 22; The present embodiment osmos tube has two, and wherein, osmos tube 121 is filled toluene, and osmos tube 122 is filled normal hexane; The calibrating gas that forms is the mixed gas of toluene, normal hexane and sample gas;
25 ℃ of holding temperatures are constant, change the flow of sample gas, the concentration of gas in can changing; As being 30ml/min with flow set, then the Dui Ying interior gas toluene and the concentration of normal hexane are respectively 116ppb and 223ppb;
Or the flow of keeping sample gas is constant, changes the temperature of permeate chamber 22, the concentration of gas in also can changing; Temperature as permeate chamber 22 is set to 40 ℃, and then the permeability of toluene and normal hexane is respectively 36nm/min and 65ng/min, and corresponding interior gas concentration is respectively 490ppb and 880ppb;
The analytical equipment of present embodiment is mounted in the portable chromatograph, and overlaps temperature conditioning unit and flow controlling unit with chromatograph shared;
Described portable chromatograph comprises sampling module, sample introduction module 5, analysis module 6 and control module, and control module comprises temperature conditioning unit 32 and flow controlling unit 42;
Described sampling module is the permeate chamber unit, and permeate chamber 22 links to each other with sample introduction module 5;
Sampling module is that gas air to be analyzed is from analyzing the sample introduction module 5 of collection in worksite to analytical instrument with sample gas;
Sample introduction module 5 comprises quantitative ring 501, sampling valve 502 and sampling pump 503, sample introduction module 5 carries out deciding the volume sampling by sampling pump 503, the repeatability of each sampling can be guaranteed,, the gas that quantitatively encircles in 501 analysis module 6 can be charged into by the switching of sampling valve 502;
Described analysis module 6 comprises chromatographic column 601, detecting device 602 and processing unit 603; 601 pairs of samples that enter of chromatographic column separate, and detecting device 602 detects the information that obtains sample, and sample signal is passed to processing unit 603, obtains the composition and the concentration information of sample;
In the present embodiment, sample gas mixes calibrating gas that the back forms and is passed in the quantitative ring 501 in the sample introduction module 5 by sampling module with interior gas, switching by sampling valve 502, calibrating gas in the quantitative ring 501 enter chromatographic column 601 to be separated, record the information of sample gas by detecting device 602, and transmit it to processing unit 603, obtain the information that sample gas is gas air to be analyzed;
The temperature of 32 pairs of permeate chamber of temperature conditioning unit 2 and quantitative ring 501, chromatographic column 601 is controlled; Flow controlling unit 42 control sample airshed and nebulizer gas pressures; By temperature of regulating permeate chamber 2 and the concentration that the sample airshed is regulated the calibrating gas that enters sample introduction module 5.
Present embodiment also provides a kind of analytical approach, and different with embodiment 1 described analytical approach is:
In step a, provide present embodiment described analytical equipment, be applied to portable chromatograph;
In step b, by the control of temperature conditioning unit 32, the temperature of keeping permeate chamber 22 is 25 ℃, and the flow velocity of flow controlling unit 42 control sample gas is 20ml/min, and sample gas feeds permeate chamber 22, will take out of from the interior gas that osmos tube 12 evaporates, and forms calibrating gas;
In the present embodiment, 25 ℃ of holding temperatures are constant, and the sample airshed is set to 30ml/min, and then the Dui Ying interior gas toluene and the concentration of normal hexane are respectively 116ppb and 223ppb;
In step c, calibrating gas feeds the quantitative ring 501 of chromatograph, is blown into chromatographic column 601 by the carrier gas of chromatographic fractionation system subsequently, separate, record the information of sample gas by detecting device 602, and transmit it to processing unit 603, obtain the information that sample gas is gas air to be analyzed.
In the present embodiment, the generation of gas does not need extra flow controlling unit in the system, gets final product with the shared cover of chromatograph; The temperature control unit of permeate chamber can be integrated in the temperature control unit of chromatograph, has simplified system; Therefore, analytical equipment of the present utility model need not independently flow and temperature control unit, and system architecture is simple, and volume is small and exquisite, is easy to miniaturization;
Can select different osmos tubes according to demand, the component of gas expands by demand in making, and than adopting gas cylinder to realize interior calibration method, provides cost savings greatly, has simplified device;
By simple adjusting temperature or flow, can realize change to calibrating gas concentration, easy and simple to handle.
Embodiment 3
See also Fig. 3, a kind of analytical equipment, different with embodiment 2 described analytical equipments is:
Described permeate chamber unit only comprises permeate chamber 23 and temperature element 8, no heating element, and temperature element 8 directly is transferred to processing unit 613 with the temperature signal that records;
Be filled with toluene in the described osmos tube 13, the length of osmos tube is 2cm, and the permeability in the time of 25 ℃ is 26ng/min, as the temperature that records in the permeate chamber 23 is 32 ℃, can calculate permeability is 42ng/min, and according to sample airshed 20ml/min, the concentration of gas is 560ppb in obtaining;
The temperature conditioning unit 33 of portable chromatograph inside is only controlled the temperature of quantitative ring 501 and chromatographic column 601;
See also Fig. 4, because logarithm and the temperature of interior gas permeability p are linear, by the temperature of control sample airshed and measurement permeate chamber 23, the concentration of gas in can determining, and then directly analyze entering chromatographic column 601 gas separated.
The permeate chamber unit does not need temperature control unit, and a temperature element only is installed; Interior gas generation device does not need extra flow controlling unit, with the shared cover of chromatograph; Therefore, the flow controlling unit supporting with analytical equipment can omit, no temperature control unit, and system architecture is simple, and volume is small and exquisite, is easy to miniaturization.
Present embodiment also provides a kind of analytical approach, and different with embodiment 2 described analytical approachs is:
In step a, provide present embodiment described analytical equipment, be applied to portable chromatograph;
In step b, temperature element 8 is measured the temperature of permeate chamber 23 in real time, and temperature value is passed to processing unit 613;
Flow controlling unit 43 control sample gas are that the flow of gas air to be analyzed is 20ml/min;
In step c, calibrating gas feeds the quantitative ring 501 of chromatograph, is blown into chromatographic column 601 by the carrier gas of chromatographic fractionation system subsequently;
Because the permeability and the temperature of interior gas are linear, by the temperature of control sample airshed and measurement permeate chamber 23, the concentration of gas in can determining, and then directly analyze entering chromatographic column 601 gas separated;
As the temperature that record in the permeate chamber 23 are 32 ℃, and can calculate permeability is 42ng/min, and according to the flow 20ml/min of sample gas and gas air to be analyzed, the concentration of gas is 560ppb in obtaining, and then analyzes entering chromatographic column 601 gas separated.
Above-mentioned embodiment should not be construed as the restriction to the utility model protection domain.Key of the present utility model is: utilize the gas source of osmos tube as system, flow controlling unit that the employing system itself carries and temperature conditioning unit are controlled the concentration of the calibrating gas of generation.Under the situation that does not break away from the utility model spirit, any type of change that the utility model is made all should fall within the protection domain of the present utility model.
Claims (5)
1. an analytical equipment comprises flow controlling unit, it is characterized in that: also comprise permeate chamber unit and at least one osmos tube;
Described osmos tube is the gas source, and the gas that evaporates from osmos tube is interior gas;
Described permeate chamber unit comprises permeate chamber and temperature element; Described osmos tube is arranged in the permeate chamber; Described permeate chamber links to each other with the sample introduction module of sample gas and analytical instrument respectively;
The flow of described flow controlling unit control sample gas.
2. analytical equipment according to claim 1 is characterized in that: described analytical equipment also comprises heating element and temperature conditioning unit, is used for the temperature in permeate chamber heating and the adjusting permeate chamber.
3. analytical equipment according to claim 1 is characterized in that: described temperature conditioning unit and/or flow controlling unit are integrated in the analytical instrument.
4. according to claim 1 or 3 described analytical equipments, it is characterized in that: described analytical instrument is chromatogram, mass spectrum or chromatograph-mass spectrometer coupling analyser.
5. analytical equipment according to claim 1 is characterized in that: fill different chemical substances in the different osmos tubes, by changing or select gas kind in the osmos tube adjustment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200464648U CN202041512U (en) | 2010-11-19 | 2011-02-24 | Analysis device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201020633754 | 2010-11-19 | ||
| CN201020633754.8 | 2010-11-19 | ||
| CN2011200464648U CN202041512U (en) | 2010-11-19 | 2011-02-24 | Analysis device |
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| CN202041512U true CN202041512U (en) | 2011-11-16 |
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| CN2011200464648U Expired - Fee Related CN202041512U (en) | 2010-11-19 | 2011-02-24 | Analysis device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183595A (en) * | 2010-11-19 | 2011-09-14 | 聚光科技(杭州)股份有限公司 | Analysis method and device |
| CN107913608A (en) * | 2017-11-10 | 2018-04-17 | 中国人民解放军陆军防化学院 | Air distributing device and air distributing method |
| CN109738579A (en) * | 2018-11-13 | 2019-05-10 | 中国航天员科研训练中心 | A kind of standard gas generating apparatus based on osmos tube |
| CN109991344A (en) * | 2019-04-04 | 2019-07-09 | 深圳博沃智慧科技有限公司 | A kind of surrounding air and the management method of the continuous online monitoring data processing of water body VOCs |
| CN112462000A (en) * | 2020-11-17 | 2021-03-09 | 广东电网有限责任公司电力科学研究院 | Gas mixing device for internal standard method |
-
2011
- 2011-02-24 CN CN2011200464648U patent/CN202041512U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183595A (en) * | 2010-11-19 | 2011-09-14 | 聚光科技(杭州)股份有限公司 | Analysis method and device |
| CN107913608A (en) * | 2017-11-10 | 2018-04-17 | 中国人民解放军陆军防化学院 | Air distributing device and air distributing method |
| CN107913608B (en) * | 2017-11-10 | 2024-01-02 | 中国人民解放军陆军防化学院 | Air distribution device and air distribution method |
| CN109738579A (en) * | 2018-11-13 | 2019-05-10 | 中国航天员科研训练中心 | A kind of standard gas generating apparatus based on osmos tube |
| CN109991344A (en) * | 2019-04-04 | 2019-07-09 | 深圳博沃智慧科技有限公司 | A kind of surrounding air and the management method of the continuous online monitoring data processing of water body VOCs |
| CN109991344B (en) * | 2019-04-04 | 2021-06-15 | 深圳博沃智慧科技有限公司 | Management method for continuous online monitoring data processing of VOCs (volatile organic compounds) in ambient air and water |
| CN112462000A (en) * | 2020-11-17 | 2021-03-09 | 广东电网有限责任公司电力科学研究院 | Gas mixing device for internal standard method |
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: ZHEJIANG FOCUSED PHOTONICS DETECTION TECHNOLOGY SE Free format text: FORMER OWNER: FOCUSED PHOTONICS (HANGZHOU) INC. Effective date: 20140514 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20140514 Address after: Hangzhou City, Zhejiang province Binjiang District 310052 shore road 760 Building 1 floor B block 6 Patentee after: Zhejiang spotlight Detection Technology Service Co., Ltd. Address before: Hangzhou City, Zhejiang province Binjiang District 310052 shore road 760 Patentee before: Focused Photonics (Hangzhou) Inc. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111116 Termination date: 20180224 |