CN103900926A - Detection analysis method for asphalt volatile organic compound - Google Patents
Detection analysis method for asphalt volatile organic compound Download PDFInfo
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- CN103900926A CN103900926A CN201410078288.4A CN201410078288A CN103900926A CN 103900926 A CN103900926 A CN 103900926A CN 201410078288 A CN201410078288 A CN 201410078288A CN 103900926 A CN103900926 A CN 103900926A
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Abstract
The invention discloses a detection analysis method for an asphalt volatile organic compound (VOC). The detection analysis method adopts a combination manner of thermogravimetry-mass spectrometry (TG-MS) to directly carry out mass spectrometry on volatile gas in the procedure temperature controlling heating process during the operation of carrying out a thermal weight loss test on asphalt. The mass of an asphalt sample is 5-10mg. The program temperature control in the thermal weight loss testing process is raised to 250 DEG C at the speed of 10 DEG C/minute. The mass spectrometry adopts molecular weight scanning with the molecular weight from 0 to 300. A TG-MS coupled technology can be used for simultaneously determining the quality change of the asphalt and qualitatively and quantitatively analyzing the VOC in a heating state of the asphalt material and the escaping quantities of the VOCs of the different asphalt can be balanced; the relatively direct reference is provided for an asphalt VOC inhibitor researcher through determining VOC components, and the inhibition condition an asphalt VOC inhibitor of on the VOC can also be directly responded, so that the emission of the asphalt VOC is reduced.
Description
Technical field
The invention belongs to hot technical field of analysis and detection, be specifically related to the determination method of a kind of pitch volatile organic matter (VOC).
Background technology
Global energy anxiety and climate change have become the significant problem of international community's common concern, and energy-saving and emission-reduction have become the corporation responsibility of international community.China, as maximum in the world developing country, becomes the object of global concern just day by day.Formed the asphalt-based material of complex mixture by different molecular weight organic hydrocarbon, in the military service process of normal temperature and pressure, can produce volatile organic compound (being pitch VOC).Bituminous pavement high-temperature heating or illumination (infrared ray, ultraviolet ray etc.) effect can promote the release of pitch VOC, and its VOC discharge capacity accounts for 25% left and right of national VOC total amount.
Pitch is in long service process, all to discharge pitch volatile organic compounds (volatile organic compounds at high-temperature heating conditioned disjunction; VOC), as phenols (phenol, cresols, naphthols etc.), phenyl ring class (dimethylbenzene, Benzpyrene, benzanthrene etc.), pyridines (pyridine, pyrimidine etc.), anthracene naphthalene class (fluoranthene, benzofluoranthrene etc.), multiring aromatic hydrocarbon (luxuriant and rich with fragrance, bend etc.) etc.
Mostly current analysis and detection method are adopt vapor-phase chromatography (GC) or with mass spectrometer coupling (GC/MS), the multiring aromatic hydrocarbon substance in glance coal carried out to qualitative or quantitative test.GC separation efficiency is high, analysis speed is fast, amount of samples is few, detection sensitivity is high, but need to select different detecting devices according to the composition characteristic of pitch volatile substance, and need could carry out qualitative and quantitative analysis to target substance with standard substance contrast.But the definite of instrument and equipment costliness and analysis condition is that choosing of chromatographic column is more difficult.The detection analysis and research of the pitch volatilization flue gas that China had carried out are in the last few years mainly the volatilization degree that adopts fluorophotometer and UV, visible light spectrometer to detect the total content of multiring aromatic hydrocarbon in glance coal to evaluate pitch.For above problem, the existing analysis to the pitch volatile matter producing under hot conditions is mainly the target substance for tool carcinogenicity in glance coal, but the analytical procedure more complicated of these target substances, and it is higher to carry out pretreated some solvent toxicity, also be there is to pollution in environment, such as need to first separating PAHs concentrate to the analysis of palycyclic aromatic (PAHs) composition, the complex steps time is long, error is large.High performance liquid chromatography (HPLC) is efficient analytical technology fast, can be suitable in principle higher boiling, poor heat stability, organism that relative molecular weight is large.But the scope of measuring has limitation, is confined to the organism that molecular weight is large.
Due to the diversity in pitch kind and source, the also more complicated of glance coal composition of generation, so the analytical approach still not stipulating for pitch volatile matter at present, also ununified standard criterion is evaluated volatilization ability and the volatilization degree of pitch.Meanwhile, the polytrope of environmental factor and the limitation of detection technique have also increased the difficulty that pitch volatile matter is detected to analysis.
Summary of the invention
The object of the invention is to provide the determination method of a kind of coupling thermal weight loss test (TG) with mass spectrometry (MS), kind and the amount of the analysis pitch volatile organic matter of quantitative and semi-quantitative for the test of pitch volatile organic matter.
The determination method of pitch volatile organic matter, is characterized in that adopting TG-MS combination (TG-MS), detects the variation of asphalt quality and the composition of VOC gas in the time pitch being carried out to the temperature programmed control heating process of thermal weight loss test.
Press such scheme, asphalt sample quality is 5-10mg.
Press such scheme, thermal weight loss test process temperature programmed control is raised to 250 ℃ from room temperature with 10 ℃/min.
Press such scheme, mass spectrophotometry adopts the molecular weight scanning of molecular weight 0 to 300.
The determination method of above-mentioned pitch volatile organic matter, adds the inhibition situation to VOC after pitch in order to detect different pitches VOC inhibitor.
The determination method of above-mentioned pitch volatile organic matter, in order to detect the variation of different molecular quantity of material burst size in temperature-rise period.
In synthetic or decomposable process, polymkeric substance, often in a kind of molten state, produces mass change and emergent gas in this process, and pitch, as a kind of polymkeric substance of complexity, in heating or ageing process, all has VOC and overflows.TG-MS technology can detect the variation of asphalt quality and the composition of VOC gas in asphalt heating simultaneously, TG tester covers the broad temperature range of-150 ℃ to 2000 ℃, guaranteeing that (0.1 μ g) has broad TG range of weighing (35g) in situation to high-res, MS instrument mass range can reach 1amu-300amu, ion gun is electron collision, and energy can reach 100eV.Therefore, utilize TG-MS combined instrument can under heated condition, detect lhv gas effusion situation of change.
Beneficial effect of the present invention:
TG-MS coupling technique can be measured mass change and the qualitative and quantitative analysis VOC of pitch under the state of asphalt material heating simultaneously, can weigh the quantity that different pitches VOC overflows, and the pitch VOC inhibitor researcher that is defined as by VOC composition provides more direct reference, also can directly react the inhibition situation of pitch VOC inhibitor to VOC, reduce the discharge of pitch VOC.
Accompanying drawing explanation
Accompanying drawing 1: embodiment 1 medium pitch is the mass change figure in temperature-rise period before and after adding VOC inhibitor;
Different molecular quantity of material burst size variation diagram in temperature-rise period in accompanying drawing 2: embodiment 2;
Accompanying drawing 3: embodiment 3 molecular weight are the mass spectrogram of 98 materials;
Accompanying drawing 4: embodiment 3 molecular weight are that 98 material cracking molecular weight are 41,55 and 69 distribution plan.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
The determination method of pitch volatile organic matter, it adopts TG-MS combination (TG-MS), detects the variation of asphalt quality and the composition of VOC gas in the time pitch being carried out to the temperature programmed control heating process of thermal weight loss test.
Pitch VOC analytic sample quality is 5-10mg.
Thermal weight loss test process temperature programmed control is raised to 250 ℃ from room temperature with 10 ℃/min.
Mass spectrophotometry adopts the molecular weight scanning of molecular weight 0 to 300.
The determination method of above-mentioned pitch volatile organic matter, adds the inhibition situation to VOC after pitch in order to direct-detection different pitches VOC inhibitor.Can also be in order to detect the variation of different molecular quantity of material burst size in temperature-rise period.TG-MS coupling technique can be measured mass change and the qualitative and quantitative analysis VOC of pitch under the state of asphalt material heating simultaneously, can weigh the quantity that different pitches VOC overflows, and the pitch VOC inhibitor researcher that is defined as by VOC composition provides more direct reference, also can directly react the inhibition situation of pitch VOC inhibitor to VOC, reduce the discharge of pitch VOC.
The brand-new synchronous TG-DSC thermal analyzer of releasing of STA449F3Jupiter Shi Naichi company, cover the broad temperature range of-150 ℃ to 2000 ℃, guaranteeing that (0.1 μ g) possesses broad TG range of weighing (35g) in situation to high-res, NETZSCH QMS403C quadrupole mass spectroscope, mass range is 1amu-300amu, ion gun is electron collision, and energy reaches 100ev.
Embodiment 1
Choose PJ90 matrix pitch and the PJ90 modified bitumen 5-10mg that adds 3% activated charcoal, heating rate control is 10 ℃/min, be heated to 250 ℃ from room temperature and carry out thermogravimetric mass spectrophotometry, in the temperature programmed control heating process of pitch being carried out to thermal weight loss test, directly volatilization gas is carried out to mass spectrophotometry, evaluate the volatile quantity of pitch VOC by the number of mass loss.
With reference to accompanying drawing 1, result shows, under the same terms, the mass loss rate of matrix pitch is 3.54%, and adds after 3% activated charcoal, and mass loss rate only has 2.45%, can find by contrast, and activated charcoal to the inhibition of pitch clearly.By thermogravimetric method, can quantitative test go out the volatilization that pitch in use exists, and also can go out the inhibition evaluation of inhibitor to pitch by comparative analysis.
Embodiment 2
By TG-MS combination instrument, matrix pitch PJ90 is tested, test condition is to carry out thermogravimetric mass spectrophotometry with the speed of 10 ℃/min from room temperature to 250 ℃, carries out mass spectrophotometry by the ion channel that various molecular weight is set.
With reference to accompanying drawing 2, the TG-MS figure of PJ90 pitch, ordinate is ionic strength, under the prerequisite of same test mass, the quality of the size of ionic strength and material volatilization is the relation of a direct ratio, result shows, the mass change trend of the volatilization of these 6 kinds of different molecular weights is basic identical, in the interval of 0-300, all there is release, and the variation that is all quality after 250 degree is just very large, than other four kinds of releasers, molecular weight is that 98.05 and 128.05 bitumen flue gas burst size is more more.
The full mass spectrum ion histogram of PJ90 in the time of 180 ℃, with reference to accompanying drawing 3,4, what Fig. 3 marked is that molecular weight is 98 mass spectrogram, and horizontal ordinate is molecular weight, and ordinate is ionic strength.Fig. 4 is that molecular weight is that 98 material cracking molecular weight are 41,55 and 69 distribution plan
Ionic strength that in Fig. 3, molecular weight is relatively little is obvious must be greater than the ion that molecular weight is larger, and this is that cracking rearrangement etc. may occur the effect ion that the various ions that evaporate from thermogravimetric instrument are subject to electric field because in mass spectrometer.Fig. 4 be exactly the molecular weight the chosen cracking molecular weight that is 98 be 41,55 and 69 distribution plan.Going out a methyl by cracking and obtained the material that molecular weight is 83, is 41,55,69 by the molecular weight of material that α-Cleavage in layer finally obtains below.
Claims (6)
1. the determination method of pitch volatile organic matter, is characterized in that adopting TG-MS combination, detects the variation of asphalt quality and the composition of VOC gas in the time pitch being carried out to the temperature programmed control heating process of thermal weight loss test.
2. the detection method of pitch volatile organic matter as claimed in claim 1, is characterized in that described asphalt sample quality is 5-10mg.
3. the detection method of pitch volatile organic matter as claimed in claim 1, is characterized in that thermal weight loss test process temperature programmed control is raised to 250 ℃ from room temperature with 10 ℃/min.
4. the detection method of pitch volatile organic matter as claimed in claim 1, is characterized in that mass spectrophotometry adopts the molecular weight scanning of molecular weight 0 to 300.
5. the determination method of pitch volatile organic matter described in claim 1, adds the inhibition situation to VOC after pitch in order to direct-detection different pitches VOC inhibitor.
6. the determination method of pitch volatile organic matter described in claim 1, in order to the variation of different molecular quantity of material burst size in temperature-rise period in direct-detection pitch.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106353217A (en) * | 2016-08-12 | 2017-01-25 | 泉州市旭丰粉体原料有限公司 | Odor test method |
| CN107576589A (en) * | 2017-08-25 | 2018-01-12 | 南京林业大学 | A kind of method evaluated age resister and influenceed on pitch short ageing |
| CN108318368A (en) * | 2017-01-17 | 2018-07-24 | 北新集团建材股份有限公司 | A kind of method of content of organics in quantitative measurment gypsum |
| CN111307649A (en) * | 2020-03-12 | 2020-06-19 | 北京市环境保护科学研究院 | Method for detecting content of volatile organic compounds in asphalt |
| CN111724868A (en) * | 2020-05-06 | 2020-09-29 | 嘉兴汇智诚电子科技有限公司 | VOC (volatile organic compound) odor rating model and optimization method |
| CN112748149A (en) * | 2020-12-23 | 2021-05-04 | 重庆交通建设(集团)有限责任公司 | Asphalt content detection method |
| CN113109203A (en) * | 2021-03-26 | 2021-07-13 | 深圳海关玩具检测技术中心 | Detection apparatus for VOC material in toy paint |
| CN113405938A (en) * | 2021-06-21 | 2021-09-17 | 广东凯金新能源科技股份有限公司 | Method for detecting content of coating layer on surface of graphite negative electrode material of lithium battery |
| CN113686945A (en) * | 2021-07-23 | 2021-11-23 | 长安大学 | Rapid analysis and detection system and method for volatile organic compounds in asphalt flue gas |
| CN114019074A (en) * | 2021-10-26 | 2022-02-08 | 武汉理工大学 | Quantification method for VOCs composition and emission amount of asphalt pavement construction site |
| CN114112782A (en) * | 2021-11-12 | 2022-03-01 | 武汉理工大学 | Method for evaluating influence degree of different flame retardants on asphalt flame-retardant and smoke-suppression effect |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN107576589A (en) * | 2017-08-25 | 2018-01-12 | 南京林业大学 | A kind of method evaluated age resister and influenceed on pitch short ageing |
| CN111307649A (en) * | 2020-03-12 | 2020-06-19 | 北京市环境保护科学研究院 | Method for detecting content of volatile organic compounds in asphalt |
| CN111724868A (en) * | 2020-05-06 | 2020-09-29 | 嘉兴汇智诚电子科技有限公司 | VOC (volatile organic compound) odor rating model and optimization method |
| CN112748149A (en) * | 2020-12-23 | 2021-05-04 | 重庆交通建设(集团)有限责任公司 | Asphalt content detection method |
| CN113109203A (en) * | 2021-03-26 | 2021-07-13 | 深圳海关玩具检测技术中心 | Detection apparatus for VOC material in toy paint |
| CN113405938A (en) * | 2021-06-21 | 2021-09-17 | 广东凯金新能源科技股份有限公司 | Method for detecting content of coating layer on surface of graphite negative electrode material of lithium battery |
| CN113686945A (en) * | 2021-07-23 | 2021-11-23 | 长安大学 | Rapid analysis and detection system and method for volatile organic compounds in asphalt flue gas |
| CN114019074A (en) * | 2021-10-26 | 2022-02-08 | 武汉理工大学 | Quantification method for VOCs composition and emission amount of asphalt pavement construction site |
| CN114112782A (en) * | 2021-11-12 | 2022-03-01 | 武汉理工大学 | Method for evaluating influence degree of different flame retardants on asphalt flame-retardant and smoke-suppression effect |
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Application publication date: 20140702 |