CN105606745A - Detection method for odor substances in exhaust gas of perfume and essence industry - Google Patents
Detection method for odor substances in exhaust gas of perfume and essence industry Download PDFInfo
- Publication number
- CN105606745A CN105606745A CN201510851518.0A CN201510851518A CN105606745A CN 105606745 A CN105606745 A CN 105606745A CN 201510851518 A CN201510851518 A CN 201510851518A CN 105606745 A CN105606745 A CN 105606745A
- Authority
- CN
- China
- Prior art keywords
- detection method
- extraction
- gas
- sample
- exhaust gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a detection method for odor substances in exhaust gas of the perfume and essence industry. According to the invention, exhaust gas discharged by the perfume and essence industry is directly or indirectly acquired, then solid-phase micro-extraction (SPME) or solid-phase adsorption-thermal desorption technology are employed for extraction of a sample; and extraction temperature and extraction time are adjusted and GC-MC is cooperatively used for analysis of the exhaust gas sample. The detection method is high in efficiency, simple to operate and applicable to analysis of odor substances with any concentration. An airbag method and negative pressure sampling technology are cooperatively used, an appropriate sampling point is selected and a representative gas sample is acquired, so original information of the sample is maintained to a greatest extent. A sampling bag has good airtightness, and a sample in the bag can be maintained for more than one month. SPME pretreatment technology is employed, so the advantages of greenness, rapidness, no pollution and repeated usability can be obtained. The detection method is applicable to both exhaust gas discharged in the perfume and essence industry and to detection of exhaust gas of industries like petroleum, the chemical industry, food, medicine and cosmetics.
Description
Technical field
The present invention relates to odor detection technology, specifically, relate to a kind of spices and essence industry uselessThe detection method of odoring substance in gas.
Background technology
In the waste gas of spices and essence industry discharge, often contain peculiar smell or odorant pollutant, these haveMachine volatile contaminant tends to stimulate people's olfactory organ, causes people's mood unhappiness,And and then affect quality of life and healthy. Except ammonia and hydrogen sulfide, the overwhelming majority has tasteGas belong to volatile organic content, these compound boiling points are lower, be easily diffused in atmosphere,Because the olfact of most of organic exhaust gas is lower, therefore the measure of its pollution prevention is requiredHeight, research shows that odorant clearance reaches 90%, the foul smell that people's sense of smell is felt is denseDegree but can only reduce half, and this causes peculiar smell or stink to be processed than other atmosphere pollution difficulties.Therefore invent a kind of method that in spices and essence industry waste gas, odoring substance detects that is applicable to, not onlySignificant to monitoring air quality, be also the prevention of odoring substance in follow-up waste gas simultaneouslyData and the theory support of science are provided with processing.
Generally speaking, the compound in spices and essence industry waste gas, a part is waved from havingSend out the raw material of property, another part is from production and the process of product. Smell thing in waste gasMatter complicated component and concentration difference are remarkable, adopt traditional solvent absorption, not only complicated operation,Waste time and energy, and easily cause secondary pollution.
In current waste gas, the analytical instrument of volatile organic matter mainly contains: gas chromatograph,High performance liquid chromatograph and gas-matter or liquid-matter instrument etc. Although may be used to volatile materialsDetection, but two kinds of analytical instrument all need to be after sample pretreatment, side can analyzeDetect. Be generally only 10 with the liquid chromatographic detection limit of UV-detector-6Though, gas-chromatographySo highly sensitive, but in waste gas except odoring substance, contain O simultaneously2、CO2And H2ODeng, even if therefore gaseous sample can not directly be brought analysis, and need to be by before rationalTreatment technology.
SPME is a kind of Sample Pretreatment Technique, has both been suitable for trace or trace in solutionThe extraction of material, is also applicable to the extraction of target compound in gaseous sample simultaneously. Extraction processWithout solvent, it is a kind of Sample Pretreatment Technique of green non-pollution. At present, SPME technologyBe widely used in the analyzing and testing of environment, food and medicine. But capable for spices and essenceThe detection of odoring substance in industry waste gas, does not still have systematic method to set up. Therefore, be necessary to buildVertical a kind of detection method for spices and essence industry waste gas odoring substance, is conducive to for spicesThe foundation of essence industry waste gas emission standard provides scientific basis, is environmental protection and air qualityControl provides data supporting.
Summary of the invention
The defect existing in order to overcome above-mentioned prior art, the object of the present invention is to provide oneCollect, extract and analyze the detection side of odoring substance in the spices and essence industry waste gas being integratedMethod.
For realizing object of the present invention, the technical scheme adopting is: with negative pressure method-gas sample bagFor sample collection method, with SPME (SPME) to target components enrichment, by excellentChange extraction time and temperature, analyze in conjunction with GC/MS, obtain a series of compounds, rightKnown compound is retrieved, and the composition that tool compound odorous can be regarded as waste gas smell becomesPoint.
In spices and essence industry waste gas, a detection method for odoring substance, directly or indirectly adoptsThe waste gas of collection spices and essence industry discharge, uses SPME (SPME) or solid phase adsorptionThermal desorption technology extracts sample, by adjusting extraction temperature and extraction time combinationGC-MS analyzes waste gas sample.
In above-mentioned detection method, described direct or indirect sampling method, comprise gas sampling method,Solid absorption method or solution absorption method.
In above-mentioned detection method, adopt SPME (SPME) or solid phase adsorption heat de-When attached technology extraction sample, extraction temperature is applicable to-50～200 DEG C, extraction time 1s～100h。
In above-mentioned detection method, the middle gas collecting of described direct or indirect gas sampling method holdsDevice comprises: gas sampling bag, gas sampler, Soviet Union's agate tank or head space bottle.
In above-mentioned detection method, the gas sampling bag in described direct or indirect gas sampling methodMaterial be PVF film, pvdf membrane, aluminum-plastic composite membrane, Devex film or fep film.
In above-mentioned detection method, the gas sampler in described direct or indirect gas sampling methodMaterial be glass or stainless steel.
In above-mentioned detection method, described solid absorption method comprises: charcoal absorption, molecular sieveAbsorption or diatomite.
In above-mentioned detection method, described solution absorption method comprises: the aqueous solution absorbs or is organic moltenAgent absorbs.
In above-mentioned detection method, adopt SPME (SPME) technology extraction waste gas,Solid-phase micro-extraction coating be PDMS, PDMS-DVB, PDMS-DVB-CAR, PA andOne in CAR-PDMS.
In above-mentioned spices and essence industry waste gas of the present invention in the detection method of odoring substance, waste gasThe qualitative basis source of middle odoring substance is in NIST database, sample raw material information and GBT14156-2009 Classification and code of flavouring substances, finally determines each compound in waste gasSmell and function.
Compared with prior art, the present invention has following beneficial effect:
1. detection method efficiency of the present invention is high, simple to operate, is applicable to analyzing any concentration odoring substance.
2. the present invention adopts airbag method in conjunction with negative pressure Sampling techniques, by selecting suitable sampled point, adoptsGet representative sample gas, to greatest extent keeping sample raw information. Sampler bag gasClose property is good, more than in bag, sample retention time can reach January.
3. in the inventive method, adopt SPME pretreatment technology, green, quick, pollution-free and can be manyInferior reusing (suggestion access times: 100 times).
4. it is up to standard that the present invention has overcome the gas discharging running into when environment department is detected, but scent of stillProblem, to a certain extent for the theory that the detection of odoring substance in waste gas has proposed science is complied withAccording to.
5. the scope of application of the present invention is not limited only to the waste gas of spices and essence industry discharge, is also applicable to simultaneouslyWaste gas in the industries such as oil, chemical industry, food, medicine and cosmetics detects.
Brief description of the drawings
Fig. 1 is odoring substance testing process in waste gas;
Fig. 2 is the waste gas material total ion current figure of first company;
Fig. 3 is the waste gas material total ion current figure of company B;
Fig. 4 is the third waste gas material total ion current figure of company;
Fig. 5 is the surrounding environment waste gas total ion current figure of fourth company.
Detailed description of the invention
Below in conjunction with embodiment, patented method of the present invention is described further, but in the present inventionThe detection method of mentioning is not only applicable to spices and essence industry, is applicable to other industry yet.
Embodiment 1: the detection of odoring substance in first essence and flavoring agent company waste gas, first to airbagDo skip test, then select volume 2L, PVF material sampler bag is collected gas sample, selectsSample 1h in the SPME probe extraction sampler bag of CAR-PDMS-DVB coating, and at GCInjection port desorb 2min. Gas chromatography-mass spectrometry analysis condition is: chromatographic column: Rtx-5, sample introduction1uL, 260 DEG C of injector temperatures, ion source temperature is 230 DEG C, split ratio is 10:1, streamSpeed lmL/min. Temperature programming: 40 DEG C of initial temperatures, keep 2min, with 5 DEG C/minSpeed be warmed up to 200 DEG C, keep 5min. Scanning of the mass spectrum scope is 40-400m/z. UselessIn gas, odoring substance testing process, as Fig. 1, detects GC/MS total ion current figure as shown in Figure 2,In waste gas, odor compound is as shown in table 1.
Embodiment 2: in second spices and essence company waste gas, odoring substance detects, and first airbag is doneSkip test, then selects volume 2L, and the sampler bag of PVDF material is collected gaseous sample,Select the SPME probe of PDMS coating to extract sample 1h in sampler bag, and at GC sample introductionMouth desorb 2min, gas chromatography-mass spectrometry analysis condition is: chromatographic column: Rtx-5, sample introduction 1uL,260 DEG C of injector temperatures, ion source temperature is 230 DEG C, split ratio is 10:1, flow velocity lML/min. Temperature programming: 40 DEG C of initial temperatures, keep 2min, with the speed of 5 DEG C/minRate is warmed up to 200 DEG C, keeps 5min, and scanning of the mass spectrum scope is 40-400m/z. Waste gasCompound total ion current figure as shown in Figure 3.
In 3: the third petro-chemical corporation's waste gas of embodiment, the detection of odoring substance, first does sky to airbagWhite test, then selects volume 2L, and the sampler bag of FEP material is collected gas sample, selectsSample 1h in the SPME probe extraction sampler bag of PDMS-DVB coating, and at GC sample introductionMouth desorb 2min, gas chromatography-mass spectrometry analysis condition is: chromatographic column: Rtx-5, sample introduction 1uL,260 DEG C of injector temperatures, ion source temperature is 230 DEG C, split ratio is 50:1, flow velocity lMl/min. Temperature programming: 60 DEG C of initial temperatures, keep 2min, with the speed of 6 DEG C/minRate is warmed up to 210 DEG C, keeps 5min, and scanning of the mass spectrum scope is 40-400m/z. Waste gasCompound total ion current figure, as shown in Figure 4.
Embodiment 4: fourth company surrounding environment foul gas detects, first does blank survey to airbagExamination, then selects volume 2L, and the sampler bag of PVF material is collected gas sample, selectsSample 6h in the SPME probe extraction sampler bag of CAR-PDMS coating, and at GC sample introductionMouth desorb 2min, gas chromatography-mass spectrometry analysis condition is: chromatographic column: Rtx-5, sample introduction 1uL,260 DEG C of injector temperatures, ion source temperature is 230 DEG C, split ratio is 10:1, flow velocity lML/min. Temperature programming: 60 DEG C of initial temperatures, keep 2min, with the speed of 8 DEG C/minRate is warmed up to 220 DEG C, keeps 5min, and scanning of the mass spectrum scope is 40-400m/z. Detect uselessCompound total ion current figure in gas, as shown in Figure 5.
Odoring substance in the waste gas of table 1 first spices and essence company discharge
Claims (9)
1. the detection method of odoring substance in a spices and essence industry waste gas, it is characterized in that directly or indirectly gathering the waste gas of spices and essence industry discharge, use SPME or solid phase adsorption thermal desorption technology to extract sample, waste gas sample is analyzed in conjunction with GC-MS by adjusting extraction temperature and extraction time.
2. detection method as claimed in claim 1, is characterized in that, described direct or indirect sampling method, comprises gas sampling method, solid absorption method or solution absorption method.
3. detection method as claimed in claim 1, is characterized in that, while adopting SPME or solid phase adsorption thermal desorption technology extraction sample, extraction temperature is applicable to-50 ~ 200 DEG C, extraction time 1s ~ 100h.
4. detection method as claimed in claim 2, is characterized in that, the middle gas collecting container of described direct or indirect gas sampling method comprises: gas sampling bag, gas sampler, Soviet Union's agate tank or head space bottle.
5. detection method as claimed in claim 2, is characterized in that, the material of the gas sampling bag in described direct or indirect gas sampling method is PVF film, pvdf membrane, aluminum-plastic composite membrane, Devex film or fep film.
6. detection method as claimed in claim 2, is characterized in that, the material of the gas sampler in described direct or indirect gas sampling method is glass or stainless steel.
7. detection method as claimed in claim 2, is characterized in that, described solid absorption method comprises: charcoal absorption, molecular sieve adsorption or diatomite.
8. detection method as claimed in claim 2, is characterized in that, described solution absorption method comprises: the aqueous solution absorbs or organic solvent absorbs.
9. detection method as claimed in claim 2, is characterized in that, adopts solid phase micro-extraction technique extraction waste gas, and solid-phase micro-extraction coating is the one in PDMS, PDMS-DVB, PDMS-DVB-CAR, PA and CAR-PDMS.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510851518.0A CN105606745A (en) | 2015-11-27 | 2015-11-27 | Detection method for odor substances in exhaust gas of perfume and essence industry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510851518.0A CN105606745A (en) | 2015-11-27 | 2015-11-27 | Detection method for odor substances in exhaust gas of perfume and essence industry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105606745A true CN105606745A (en) | 2016-05-25 |
Family
ID=55986840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510851518.0A Pending CN105606745A (en) | 2015-11-27 | 2015-11-27 | Detection method for odor substances in exhaust gas of perfume and essence industry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105606745A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106731887A (en) * | 2017-01-06 | 2017-05-31 | 宁波大学 | A kind of VOCs extracts perforated membrane |
| CN106959353A (en) * | 2017-03-30 | 2017-07-18 | 河南中烟工业有限责任公司 | Tobacco aromaticss essence smells fragrant pen and smells fragrant head |
| CN107389823A (en) * | 2017-07-31 | 2017-11-24 | 江苏省环境监测中心 | The method of SPME analysis of off-flavors system detectio pickles factory uncontrollable discharge smell substance |
| CN107843682A (en) * | 2016-09-19 | 2018-03-27 | 株式会社岛津制作所 | The fault detection method and VOC continuous exhaust gas analysis devices of VOC continuous exhaust gas analysis devices |
| CN109602065A (en) * | 2018-12-14 | 2019-04-12 | 河南卷烟工业烟草薄片有限公司 | The essence and its recovery method that are recycled from reconstituted tobacco enrichment process institute waste air and application |
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN113166678A (en) * | 2019-03-13 | 2021-07-23 | 松下知识产权经营株式会社 | Information providing method, information providing system, perfume adding device, perfume detecting device and information management device |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999031480A1 (en) * | 1997-12-18 | 1999-06-24 | Varian, Inc. | Improved method and device for solid phase microextraction |
| AU5575599A (en) * | 1998-09-21 | 2000-04-10 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
| EP1406077A2 (en) * | 1999-03-26 | 2004-04-07 | Gerstel Systemtechnik GmbH & Co. KG | Collector for the solid phase microextraction and the analysis of substances |
| CN1721850A (en) * | 2004-07-14 | 2006-01-18 | 中国科学院大连化学物理研究所 | A kind of solid phase extraction sample bottle and thermal analysis apparatus |
| CN1892213A (en) * | 2006-03-16 | 2007-01-10 | 中国人民解放军63977部队 | Solid-phase micro-extracting device and method in gas-sampling tube |
| CN101871921A (en) * | 2010-07-02 | 2010-10-27 | 娄大伟 | Needle type extraction device suitable for gas chromatography and using method |
| CN102062767A (en) * | 2009-11-16 | 2011-05-18 | 中国科学院大连化学物理研究所 | Online sampling, enriching, thermal desorption and chromatographic sample injection device combined device for atmospheric sample |
-
2015
- 2015-11-27 CN CN201510851518.0A patent/CN105606745A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999031480A1 (en) * | 1997-12-18 | 1999-06-24 | Varian, Inc. | Improved method and device for solid phase microextraction |
| AU5575599A (en) * | 1998-09-21 | 2000-04-10 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
| EP1406077A2 (en) * | 1999-03-26 | 2004-04-07 | Gerstel Systemtechnik GmbH & Co. KG | Collector for the solid phase microextraction and the analysis of substances |
| CN1721850A (en) * | 2004-07-14 | 2006-01-18 | 中国科学院大连化学物理研究所 | A kind of solid phase extraction sample bottle and thermal analysis apparatus |
| CN1892213A (en) * | 2006-03-16 | 2007-01-10 | 中国人民解放军63977部队 | Solid-phase micro-extracting device and method in gas-sampling tube |
| CN102062767A (en) * | 2009-11-16 | 2011-05-18 | 中国科学院大连化学物理研究所 | Online sampling, enriching, thermal desorption and chromatographic sample injection device combined device for atmospheric sample |
| CN101871921A (en) * | 2010-07-02 | 2010-10-27 | 娄大伟 | Needle type extraction device suitable for gas chromatography and using method |
Non-Patent Citations (5)
| Title |
|---|
| K.K. KLEEBERG 等: "Development of a simple and sensitive method for the characterization of odorous waste gas emissions by means of solid-phase microextraction (SPME) and GC–MS/olfactometry", 《WASTE MANAGEMENT》 * |
| 杨坪 等著: "《环境样品分析新方法及其应用 》", 31 December 2010, 北京：科学出版社 * |
| 王艳丽 等: "固相微萃取在空气有机污染物监测的应用", 《环境科学与管理》 * |
| 邓强 等: "北京市安定生活垃圾填埋场 VOCs恶臭物质及其臭气强度", 《环境科学学报HTTP://WWW.CNKI.NET/KCMS/DETAIL/11.1843.X.20150526.0902.007.HTML》 * |
| 降升平 等: "SPME-GC/MS法分析室内空气中挥发性有机物", 《太原理工大学学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107843682A (en) * | 2016-09-19 | 2018-03-27 | 株式会社岛津制作所 | The fault detection method and VOC continuous exhaust gas analysis devices of VOC continuous exhaust gas analysis devices |
| CN107843682B (en) * | 2016-09-19 | 2020-09-29 | 株式会社岛津制作所 | Fault detection method for VOC waste gas continuous analysis device and VOC waste gas continuous analysis device |
| CN106731887A (en) * | 2017-01-06 | 2017-05-31 | 宁波大学 | A kind of VOCs extracts perforated membrane |
| CN106959353A (en) * | 2017-03-30 | 2017-07-18 | 河南中烟工业有限责任公司 | Tobacco aromaticss essence smells fragrant pen and smells fragrant head |
| CN107389823A (en) * | 2017-07-31 | 2017-11-24 | 江苏省环境监测中心 | The method of SPME analysis of off-flavors system detectio pickles factory uncontrollable discharge smell substance |
| CN109602065A (en) * | 2018-12-14 | 2019-04-12 | 河南卷烟工业烟草薄片有限公司 | The essence and its recovery method that are recycled from reconstituted tobacco enrichment process institute waste air and application |
| CN109602065B (en) * | 2018-12-14 | 2022-03-01 | 河南卷烟工业烟草薄片有限公司 | Essence recovered from waste gas discharged in reconstituted tobacco concentration process and recovery method and application thereof |
| CN113166678A (en) * | 2019-03-13 | 2021-07-23 | 松下知识产权经营株式会社 | Information providing method, information providing system, perfume adding device, perfume detecting device and information management device |
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105606745A (en) | Detection method for odor substances in exhaust gas of perfume and essence industry | |
| Munoz et al. | Monitoring techniques for odour abatement assessment | |
| Zhang et al. | Field air sampling and simultaneous chemical and sensory analysis of livestock odorants with sorbent tubes and GC–MS/olfactometry | |
| Giungato et al. | Synergistic approaches for odor active compounds monitoring and identification: State of the art, integration, limits and potentialities of analytical and sensorial techniques | |
| Woolfenden | Thermal desorption gas chromatography | |
| Shang et al. | Rapid determination of volatile constituents of Michelia alba flowers by gas chromatography–mass spectrometry with solid-phase microextraction | |
| Sironi et al. | Continuous monitoring of odours from a composting plant using electronic noses | |
| Kamarulzaman et al. | Identification of VOCs from natural rubber by different headspace techniques coupled using GC-MS | |
| Hopkins et al. | A two-column method for long-term monitoring of non-methane hydrocarbons (NMHCs) and oxygenated volatile organic compounds (o-VOCs) | |
| Gębicki et al. | Discrimination of selected fungi species based on their odour profile using prototypes of electronic nose instruments | |
| Borrás et al. | Determination of reduced sulfur compounds in air samples for the monitoring of malodor caused by landfills | |
| CN107290462A (en) | A kind of detection method of uncontrollable discharge volatile organic matter | |
| Gallego et al. | Development of a method for determination of VOCs (including methylsiloxanes) in biogas by TD-GC/MS analysis using Supel™ inert film bags and multisorbent bed tubes | |
| Robertson et al. | The application of thermal desorption‐gas chromatography‐mass spectrometry to the analyses of flower volatiles from five varieties of oilseed rape (Brassica napus spp. oleiferd) | |
| CN114935618B (en) | Non-target screening-based precise identification method for odor-causing substances | |
| An et al. | Frontier review on comprehensive two-dimensional gas chromatography for measuring organic aerosol | |
| Ren et al. | Quartz filter-based thermal desorption gas chromatography mass spectrometry for in-situ molecular level measurement of ambient organic aerosols | |
| Lacko et al. | Addition of fast gas chromatography to selected ion flow tube mass spectrometry for analysis of individual monoterpenes in mixtures | |
| Matz et al. | On-line monitoring of biotechnological processes by gas chromatographic-mass spectrometric analysis of fermentation suspensions | |
| CN103940939B (en) | Based on the foul gas pick-up unit of micro-fluidic chip | |
| CN203422237U (en) | Sampling device for GC-MS (gas chromatography-mass spectrometer) headspace analysis | |
| Wang et al. | Influence of sampling methods and storage condition on volatile methyl siloxanes quantification in biogas | |
| Ras et al. | Solid-phase microextraction—Gas chromatography to determine volatile organic sulfur compounds in the air at sewage treatment plants | |
| Gutiérrez et al. | Compost pile monitoring using different approaches: GC–MS, E-nose and dynamic olfactometry | |
| Muenchmeyer et al. | Improving electronic noses using a trap and thermal desorption unit |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160525 |