CN101263385A - Gas analysis method - Google Patents
Gas analysis method Download PDFInfo
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- CN101263385A CN101263385A CNA2006800335776A CN200680033577A CN101263385A CN 101263385 A CN101263385 A CN 101263385A CN A2006800335776 A CNA2006800335776 A CN A2006800335776A CN 200680033577 A CN200680033577 A CN 200680033577A CN 101263385 A CN101263385 A CN 101263385A
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Abstract
The present invention provides a method for analyzing gases such as carbon dioxide. Economical on-site analytical capabilities are provided for by concentrating the impurities prior to their analysis.
Description
Invention field
The invention provides a kind of method of analytical gas.More specifically, the invention provides a kind of method of in production and/or purge process, analyzing impurity content in the carbon dioxide.
Background of invention
Carbon dioxide is used for many industry and domestic applications, does not contain various impurity in many these application requirements carbon dioxide.Unfortunately, the carbon dioxide that obtains by natural source such as gas well, chemical method, fermentation process, the carbon dioxide that perhaps produces in commercial production particularly by the carbon dioxide of hydrocarbon products burning generation, contains sulphur compound such as the carbonyl sulfide (COS) and the sulfuretted hydrogen (H of impurity level usually
2S), oxidation product (oxygenates) is as acetaldehyde and alcohol, and aromatic compounds such as benzene.When carbon dioxide is estimated needing to be used for the application (for example manufacturing of food and soda, medical product and electron device and cleaning) of high-pureness carbon dioxide, must before using, sulphur compound and other hydrocarbon impurity that contains in the air-flow be reduced to low-down content.The Impurity removal level that requires changes according to the application of carbon dioxide.For example, for the beverage articles for use, carbon dioxide (CO
2) in total sulfur content should be lower than 0.1ppm, the content of aromatic hydrocarbon must be lower than 0.02ppm.For the electronics clean applications, the content of heavy hydrocarbon need be reduced to and be lower than 0.1ppm.
For guaranteeing that purification process can remove impurity to the content that requires, needing can be reliably and measure the analytical approach of the impurity of extremely low (ppm level and ppb level) content such as sulphur compound, aldehyde, pure and mild aromatic compounds economically.The whole bag of tricks that is used to analyze these impurity is known, comprises the gas chromatography with various detecting devices, total hydrocarbon and analysis of total sulfur device, GC/MS and some are based on infrared detecting device.Most of available analytical approach will consume tens thousand of U.S. dollars usually, and its cost is too high for many carbon dioxide production and purifier apparatus.
The invention provides a kind of easy, analytical approach effectively and cheaply, be used for analyzing various impurity in the gas of carbon dioxide and so in production, purifying and use.
Summary of the invention
The invention provides a kind of method of measuring impurity concentration in the purified gases process, this method comprises: in the air-flow feeding gas adsorbing device that a) will be impure, in room temperature or be higher than under the temperature of room temperature and keep a period of time, with the impurity in the adsorption gas flow; B) stop to flow of air-flow; C) desorption uses detecting device to analyze the air-flow of gained.
The present invention also provides a kind of analytical approach of measuring impurity concentration in the process of production and purification of carbon dioxide, this method comprises: a) impure air-flow is fed in the gas adsorbing device, in room temperature or be higher than under the temperature of room temperature and keep a period of time, with the impurity in the adsorption gas flow; B) stop to flow of air-flow; And c) desorption uses detecting device to analyze the air-flow of gained.
In one embodiment, described air-flow is a carbon dioxide gas stream.Gas adsorbing device is the filling adsorbent bed in the chromatogram.Chromatogram is a gas chromatography.Detecting device can be flame ionization detector (FID) and the photoionization detector (PID) that is used to detect hydrocarbon impurity, and the detecting device as flame photometric detector (FPD) (FPD), sulfur chemistry luminescence detector (SCD) and pulse flame photometric detector (FPD) (PFPD) and so on that is used to detect sulfocompound.
Brief Description Of Drawings
Though instructions and claims have pointed out that clearly the applicant thinks its subject matter of an invention, the present invention may be better understood in conjunction with the drawings, and wherein Fig. 1 is the detailed description of analysis platform (analytical skid).
Detailed Description Of The Invention
Usually the carbon dioxide that is used for industrial process of producing contains many impurity. These impurity usually are many The problem that Carbon Dioxide Application is concerned about, but estimating that being used for the people consumes (for example soda) and electronics system In the production of the product of making, the purity of carbon dioxide is very important, can affect taste, the matter of final products Amount and legitimacy.
Can be common by the impure carbon dioxide (impure carbon dioxide) that any carbon dioxide source obtains Contain following impurity: sulphur compound, for example carbonyl sulfide, hydrogen sulfide, dimethyl sulfide, sulfur dioxide and mercaptan; Hydrocarbon impurity, for example aldehyde, alcohol, aromatic compounds, propane, ethene; And other impurity, for example water and one Carbonoxide. The invention describes the new method of analyzing some of them impurity. Concept of the present invention is not limited to dioxy Change carbon, can be used for analyzing the impurity in other gas.
For the purposes of the present invention, analyze various in the carbon dioxide by Sulfur Analysis instrument and hydrocarbon analyzer Impurity. When other impurity in analyzing other gas such as halogenated hydrocarbons, can use other detector. For carbon dioxide, two analyzers can be in independent device, gas-chromatography for example, perhaps two Individual analyzer is independently to install. Before analyzing, various sulphur impurities and hydrocarbon impurity are concentrated, to carry High their content in sample. This step has been improved the detection lower limit of various analyzers. This particularly suitable In must be with the impurity of content to benzene below the 20ppb and so in the beverage articles for use. The method comprise with Impurity absorption had impurity to be analyzed optionally on the adsorbent several minutes. For concentrating of benzene, can To use the adsorbent of pool Parker Q (Poropak Q) and so on. Behind absorption impurity, adsorption column is added fast Heat is transported to impurity in the splitter, sends into then and carries out quantitative analysis in the detector. If use Gas-chromatography is analyzed, and adsorption column can be positioned at inside or the outside of gas chromatograph oven. For Decrease cost is preferably at GC indoor splitter and adsorption column.
Before analyzing, impurity is concentrated, can use the detecting device of lower cost to analyze various impurity.For example, in order to measure the benzene of 20ppb in the CO 2, need to use expensive photoionization detector (PID), but after sample concentration, can use the flame ionization detector (FID) of considerably cheaper.In addition, in order to detect the sulphur impurity of 20-50ppb, need to use expensive sulfur chemistry luminescence detector (SCD), but after sample concentration, can use cheap flame photometric detector (FPD) (FPD).
The sulfur analyzer device will be analyzed the total sulfur content of each operation stage or the content of various sulphur class materials.For beverage grade carbon dioxide, the total sulfur content in the product except that sulphuric dioxide must be lower than 0.1ppm, and sulphuric dioxide must be lower than 1ppm.In order to measure total sulfur content, sulphur impurity is in containing the catalytic reactor of sulfur resistant catalyst or be oxidized to sulphuric dioxide in the ozone generator based on corona discharge usually.Use sulphur specific detectors such as sulfur chemistry luminescence detector (SCD), flame photometric detector (FPD) (FPD) or pulse flame photometric detector (FPD) (PFPD) to analyze oxidation sulphuric dioxide afterwards.When needs are determined the species (speciation) of sulphur compound, can randomly concentrate sulphur impurity, be delivered directly to then in separating column and the detecting device, and from the oxidation unit bypass.
The hydrocarbon analyser will be analyzed the total hydrocarbon content (as methane) at each operation stage or the content of various hydrocarbon materials.For beverage grade carbon dioxide, require the total hydrocarbon content in the product to be lower than 50ppm, then different to the restriction of each component, for example the content of benzene needs less than 20ppb, and the content of acetaldehyde needs less than 0.1ppm, and the content of methyl alcohol needs less than 10ppm.For highly purified electronics applications, heavy hydrocarbon (＞C
3) content must be lower than 0.1ppm.In order to measure total hydrocarbon content, sample concentrator and separating column all are arranged on bypass, and sample directly is transported among the FID and measures.For the measurement of various hydrocarbon materials, sample delivery to concentrator and separating column, is transported to fid detector then, analyze.
The details of analytic system is shown among Fig. 1.In Fig. 1, pipeline 14 is the feed pipes that enter analysis platform.Pipeline 16 is guided a part of gaseous sample into multiport valve 28A by valve 18 and pipeline 26.Carrier as nitrogen and so on is introduced by pipeline 20 and valve 22, communicates with pipeline 26, mixes with gaseous sample.
Guide another part gaseous sample into pipeline 32 along pipeline 14, it and the air mixed that enters along pipeline 34 at this.This gaseous sample is introduced in optional the sulphur oxidation catalyzer or ozone generator 36, arrived multiport valve 28B by pipeline 38 then.Pipeline 39 is introduced concentrator 42B, separating column 43B and another detecting device 46 with sample.In order to detect sulphur impurity, detecting device 46 can be FPD (flame photometric detector (FPD)).Pipeline 52 is drawn from detecting device 46, and will analyze data delivery to bashertron, is transported to integraph/computing machine (not shown) then.
Among Fig. 1 valve 28A and 28B have with purge process that they link to each other in the sample that obtains of diverse location, sample position can computerized control.The impurity of different phase in like this can the monitoring process process.
In the future the signal of self-detector is converted to the concentration of various impurity by integraph and/or computing machine, and this information can be used for production operator, perhaps is transferred to central authorities control place.If impurity increases suddenly or other data readings shows the against regulation value of purity, then the operator can end or stop purge process, investigates abnormal conditions simultaneously.
Equipment of the present invention and method be design with solving carbon dioxide impurities, the carbon dioxide that provides in the operational phase of the manufacture process problem of being correlated with particularly.By carrying out purifying and analysis simultaneously, the operator of production facility can obtain stable supply and the carbon dioxide of quality assurance is arranged.
Applicable industry of the present invention or consumption industry include but not limited to the manufacturing and the cleaning of food; The manufacturing of electronic product, electronic unit and assembly; The cleaning of medical product; The carbonating of soft drink, beer and water; Contain the covering of the storage tank and the container of flammable liquid or powder; The covering of the material that in air, can degrade, for example vegetable oil, spices and essence.
Embodiment 1
Use contains the carbon dioxide sample of 1ppm benzene, this sample with the flow velocity of 50 ml/min by filled respectively activated alumina, silica gel, DAY zeolite and pool Parker Q different 2.0 " * 1/8 " (0.3 centimetre of 5 cm x) post.This post is positioned at 50 ℃ gas chromatograph oven, links to each other with fid detector.Made sample continuous flow about 10 minutes, and all do not observe benzene for any post and penetrate (breakthrough).
Stop sample flow, nitrogen passes through this post as carrier gas.In less than 1 minute, this post heating chamber is heated to 150 ℃, uses the outlet of fid detector monitoring post.Observe few benzene desorption for activated alumina, silica gel and DAY, this is because their affinity stronger to benzene.But, for pool Parker Q, in less than 1 minute time, all benzene desorption.
For pool Parker Q, the enrichment factor that obtains with respect to 1 ml sample endless tube is 500.The benzene detection lower limit of supposing fid detector is 0.5ppm, then adopts Sample Preconcentration Technique, the low 1ppb that reaches of the benzene concentration that can measure under the situation of using equality detector.This technology can be used for other impurity, for example aldehyde and alcohol.This technology can also be used for other gas and other impurity.
The present invention is specially adapted to the product of analysis part purifying or the impurity in the final products, because the content of impurity is than high-adsorption-capacity among low concentrator 42A that need not move under room temperature or higher temperature and the 42B in the air-flow.And the adsorbent in these concentrators must be weak adsorbent (for example adopting pool Parker Q for benzene), impurity easy desorption when the GC heating chamber heats like this.The strong adsorbent possibility effect of zeolite and activated alumina and so on is bad, because impurity is difficult to desorption from these strong adsorbents.
Though described the present invention with reference to plurality of embodiments and embodiment, those skilled in the art can carry out various changes, interpolation and omission under the situation that does not deviate from spirit and scope of the invention.
Claims (21)
1. method of in the purification for gas process, measuring impurity concentration, this method comprises:
A) impure air-flow is fed in the gas adsorbing device, in room temperature or be higher than under the temperature of room temperature and keep a period of time, with the impurity in the adsorption gas flow;
B) stop to flow of air-flow;
C) desorption is used the detecting device analysing impurity.
2. the method for claim 1 is characterized in that, described gas is carbon dioxide.
3. the method for claim 1 is characterized in that, described impurity is selected from H
2S, COS, dimethyl sulfide, benzene, aldehyde, short carbon chain alcohol and hydrocarbon.
4. the method for claim 1 is characterized in that, described gas adsorbing device is included in the packed bed in the gas chromatography.
5. method as claimed in claim 4 is characterized in that, described gas is by gas separating column desorption.
6. method as claimed in claim 4 is characterized in that, described gas column chromatography contains the analytical equipment of measuring organic compound impurity, and described organic compound impurity is selected from following: benzene, aldehyde, short carbon chain alcohol and hydrocarbon.
7. method as claimed in claim 4 is characterized in that, described gas chromatography is communicated with the analytical equipment of measuring sulphur compound.
8. the method for claim 1 is characterized in that, described detecting device is selected from: the flame ionization detector (FID) and the photoionization detector (PID) that are used to detect hydrocarbon impurity; Be used to detect flame photometric detector (FPD) (FPD), sulfur chemistry luminescence detector (SCD) and the pulse flame photometric detector (FPD) (PFPD) of sulfocompound.
9. analytical approach of in carbon dioxide production and purge process, measuring impurity concentration, this method comprises:
A) impure air-flow is fed in the gas adsorbing device, in room temperature or be higher than under the temperature of room temperature and keep a period of time, with the impurity in the adsorption gas flow;
B) stop to flow of air-flow;
C) desorption is used the detecting device analysing impurity.
10. method as claimed in claim 9 is characterized in that described gas is carbon dioxide.
11. method as claimed in claim 9 is characterized in that, described impurity is selected from H
2S, COS, dimethyl sulfide, benzene, aldehyde, short carbon chain alcohol and hydrocarbon.
12. method as claimed in claim 9 is characterized in that, described gas adsorbing device is included in the packed column in the gas chromatography.
13. method as claimed in claim 12 is characterized in that, described gas is by gas separating column desorption.
14. method as claimed in claim 12 is characterized in that, described gas column chromatography comprises the analytical equipment of measuring organic compound impurity, and described organic compound impurity is selected from following: benzene, aldehyde, short carbon chain alcohol and hydrocarbon.
15. method as claimed in claim 12 is characterized in that, described gas chromatography is communicated with the analytical equipment of measuring sulphur compound.
16. method as claimed in claim 9 is characterized in that, described detecting device is selected from: the flame ionization detector (FID) and the photoionization detector (PID) that are used to detect hydrocarbon impurity; Be used to detect flame photometric detector (FPD) (FPD), sulfur chemistry luminescence detector (SCD) and the pulse flame photometric detector (FPD) (PFPD) of sulfocompound.
17. a method of measuring impurity concentration in the carbon dioxide purge process, this method comprises:
A) impure carbon dioxide gas stream is fed in the packed column in chromatogram arrangement, in room temperature or be higher than under the temperature of room temperature and keep a period of time, to adsorb the impurity in this air-flow;
B) stop to flow of air-flow, the temperature of rising column chromatography device is with desorption impurity;
C) use detecting device to analyze the air-flow of gained.
18. method as claimed in claim 17 is characterized in that, described impurity is selected from H
2S, COS, dimethyl sulfide, benzene, aldehyde, short carbon chain alcohol and hydrocarbon.
19. method as claimed in claim 17, it is characterized in that, the carbon dioxide gas stream that described gas chromatography will contain impurity feeds analytical equipment, and to measure organic compound impurity, described organic compound impurity is selected from following: benzene, aldehyde, short carbon chain alcohol and hydrocarbon.
20. method as claimed in claim 17 is characterized in that, described gas chromatography comprises the analytical equipment of measuring sulphur compound.
21. method as claimed in claim 17 is characterized in that, described detecting device is selected from: the flame ionization detector (FID) and the photoionization detector (PID) that are used to detect hydrocarbon impurity; Be used to detect flame photometric detector (FPD) (FPD), sulfur chemistry luminescence detector (SCD) and the pulse flame photometric detector (FPD) (PFPD) of sulfocompound.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US70633005P | 2005-08-08 | 2005-08-08 | |
| US60/706,330 | 2005-08-08 | ||
| US11/500,131 | 2006-08-07 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648082B (en) * | 2009-08-13 | 2011-06-22 | 同济大学 | Low-temperature gathering device and low-temperature gathering method capable of realizing synchronous gathering of H2/CH4/CO2/H2S |
| CN102272591B (en) * | 2009-01-05 | 2014-06-11 | 合成化学彭特博士有限公司 | Measuring machine and method for detecting the content of oil, hydrocarbons, and oxidizable gases in air or compressed air |
| CN103913536A (en) * | 2009-07-31 | 2014-07-09 | 创控生技股份有限公司 | Equipment and method with front-end and back-end pre-concentrators and moisture removal |
| CN104458350A (en) * | 2014-12-18 | 2015-03-25 | 天津理工大学 | Gas capture concentration device and working method thereof for improving gas measurement sensitivity |
| CN104596832A (en) * | 2015-01-14 | 2015-05-06 | 成都瑞芬思生物科技有限公司 | Atmospheric haze purification method |
| US9683974B2 (en) | 2009-07-07 | 2017-06-20 | Tricorntech Corporation | Cascaded gas chromatographs (CGCs) with individual temperature control and gas analysis systems using same |
| CN107436322A (en) * | 2016-05-17 | 2017-12-05 | 株式会社堀场制作所 | Gas analyzing apparatus |
| US9921192B2 (en) | 2010-04-23 | 2018-03-20 | Tricorntech Corporation | Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis |
| CN107870113A (en) * | 2016-09-27 | 2018-04-03 | 核工业北京地质研究院 | A kind of gas purification apparatus in Ar Ar Isotope Datings test |
| CN108152219A (en) * | 2017-12-29 | 2018-06-12 | 亚申科技研发中心（上海）有限公司 | The real-time detection method and device of impurity in synthesis gas |
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| US6511528B1 (en) * | 1999-03-26 | 2003-01-28 | Uop Llc | Purification of carbon dioxide |
| WO2004077015A2 (en) * | 2003-02-21 | 2004-09-10 | Mykrolis Corporation | Method for analysis of contaminants in a process fluid stream |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102272591B (en) * | 2009-01-05 | 2014-06-11 | 合成化学彭特博士有限公司 | Measuring machine and method for detecting the content of oil, hydrocarbons, and oxidizable gases in air or compressed air |
| US9683974B2 (en) | 2009-07-07 | 2017-06-20 | Tricorntech Corporation | Cascaded gas chromatographs (CGCs) with individual temperature control and gas analysis systems using same |
| CN103913536A (en) * | 2009-07-31 | 2014-07-09 | 创控生技股份有限公司 | Equipment and method with front-end and back-end pre-concentrators and moisture removal |
| CN103913536B (en) * | 2009-07-31 | 2016-05-11 | 创控生技股份有限公司 | There is the Apparatus and method for of front end and rear end preconcentrator and dehumidifying |
| US9658196B2 (en) | 2009-07-31 | 2017-05-23 | Tricorntech Corporation | Gas collection and analysis system with front-end and back-end pre-concentrators and moisture removal |
| CN101648082B (en) * | 2009-08-13 | 2011-06-22 | 同济大学 | Low-temperature gathering device and low-temperature gathering method capable of realizing synchronous gathering of H2/CH4/CO2/H2S |
| US9921192B2 (en) | 2010-04-23 | 2018-03-20 | Tricorntech Corporation | Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis |
| US11796515B2 (en) | 2010-04-23 | 2023-10-24 | Tricorntech Corporation | Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis |
| US11035834B2 (en) | 2010-04-23 | 2021-06-15 | TricornTech Taiwan | Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis |
| CN104458350A (en) * | 2014-12-18 | 2015-03-25 | 天津理工大学 | Gas capture concentration device and working method thereof for improving gas measurement sensitivity |
| CN104596832A (en) * | 2015-01-14 | 2015-05-06 | 成都瑞芬思生物科技有限公司 | Atmospheric haze purification method |
| CN104596832B (en) * | 2015-01-14 | 2017-05-03 | 成都瑞芬思生物科技有限公司 | Atmospheric haze purification method |
| CN107436322A (en) * | 2016-05-17 | 2017-12-05 | 株式会社堀场制作所 | Gas analyzing apparatus |
| CN107870113A (en) * | 2016-09-27 | 2018-04-03 | 核工业北京地质研究院 | A kind of gas purification apparatus in Ar Ar Isotope Datings test |
| CN107870113B (en) * | 2016-09-27 | 2024-02-09 | 核工业北京地质研究院 | Gas purification device in Ar-Ar isotope dating test |
| CN108152219A (en) * | 2017-12-29 | 2018-06-12 | 亚申科技研发中心（上海）有限公司 | The real-time detection method and device of impurity in synthesis gas |
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Application publication date: 20080910 |