CN102507718A - Asphalt analysis discriminating method - Google Patents

Asphalt analysis discriminating method Download PDF

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CN102507718A
CN102507718A CN2011103281588A CN201110328158A CN102507718A CN 102507718 A CN102507718 A CN 102507718A CN 2011103281588 A CN2011103281588 A CN 2011103281588A CN 201110328158 A CN201110328158 A CN 201110328158A CN 102507718 A CN102507718 A CN 102507718A
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asphalt
molecular weight
standard specimen
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CN102507718B (en
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曹东伟
杨闯
张海燕
史权
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Research Institute of Highway Ministry of Transport
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Abstract

The invention relates to an asphalt analysis discriminating method by utilizing an electronic spray ionization Fourier transform ion cyclotron resonance mass spectrometry technology. The asphalt analysis discriminating method comprises the following steps of: (1) detecting a standard sample in an electronic spray ionization Fourier transform ion cyclotron resonance mass spectrometer to determine molecular composition, molecular weight and distributed mass spectrometric data of a polar compound in the standard sample; (2) detecting a sample to be detected in the electronic spray ionization Fourier transform ion cyclotron resonance mass spectrometer to determine the molecular composition, molecular weight and distributed mass spectrometric data of another polar compound in the sample to be detected; and (3) evaluating differences of the molecular compositions, molecular weights and distribution of the sample to be detected and the standard sample, detected in a wide band mode and a narrow band mode, by utilizing a spectral ratio method and a repeatability limit method to obtain an asphalt fingerprint identification result. Through the asphalt analysis discriminating method disclosed by the invention, the characteristics of the obtained asphalt fingerprint are remarkable and have very high representativeness and reliability; and the variety discrimination and product identification of petroleum asphalt, coal pitch, natural asphalt (consisting of rock asphalt and lake asphalt) can be realized by comparison of asphalt fingerprint mass spectrometric data of the standard sample and the sample to be detected.

Description

A kind of pitch is analyzed discrimination method
Technical field
The invention belongs to a kind of pitch fingerprint discrimination method, relate to a kind of particularly based on the mass spectral pitch analysis of Fourier Transform Ion cyclotron Resonance discrimination method.
Background technology
Pitch is a kind of complex mixture of being made up of multiple complicated high-molecular hydrocarbons and derivant thereof.Its quality quality is the construction work quality of decision bituminous pavement directly, influences the usability and the serviceable life thereof of bituminous pavement.At present; Still there is underproof asphaltic products in China pitch market; Though China has formulated ordinary road petroleum bitumen technical manual, whether qualified differentiate pitch from the rerum natura angle often, like common pitch three big indexs: pen., softening point and ductility.This classic method not only takes time and effort, and is subject to the influence of modifier and stabilizing agent, makes the test findings distortion.Therefore says that simple physical index detection can't obtain characteristic " fingerprint " information of pitch at all, also just can't be really the quality of pitch be control effectively.The risks of construction of the pavement of road that lacks method that effective asphalt quality detects and quality control and bring are also very big.Thereby developing a kind of pitch fingerprint discrimination method is that asphalt quality is controlled pressing for of field under the existing situation.
Summary of the invention
The purpose of this invention is to provide a kind of simple to operate, analyze accurately pitch and analyze discrimination method.
For realizing above-mentioned purpose, the pitch of Fourier Transform Ion cyclotron Resonance mass-spectrometric technique that utilizes provided by the invention is analyzed discrimination method, and its process is:
1) standard specimen is detected in fourier transform ion cyclotron resonance mass spectrometer, measure the mass spectrometric data of wherein polar compound molecular composition and molecular weight and distribution thereof;
2) testing sample is detected in fourier transform ion cyclotron resonance mass spectrometer, measure the mass spectrometric data of wherein polar compound molecular composition and molecular weight and distribution thereof;
3) utilize repeated limit method and spectrogram matching method to estimate the difference of testing sample and standard specimen Semi-polarity compound molecule composition and molecular weight and distribution thereof, thereby obtain identification result.
Described method, wherein, standard specimen and testing sample Semi-polarity compound molecular weight and distribution thereof are under the broadband scanning pattern, the scanning mass-to-charge ratio is the mass spectrometric data in the 150-1000 scope.
Described method, wherein, standard specimen and testing sample Semi-polarity compound molecular weight and distribution thereof are under the arrowband scan pattern, the scanning mass charge ratio range is the mass spectrometric data in the 440-460 scope.
Described method wherein, contains N in standard specimen and the testing sample polar compound 1, O 1, N 1O 1, O 2, N 2, N 1O 2, N 1S 1, O 1S 1, O 2S and N 1O 1S 1Deng heteroatoms.
Described method, wherein, the molecular weight of standard specimen and testing sample and distribution thereof are the mass spectrometric datas that is taken under the broadband scanning pattern, and signal to noise ratio (S/N ratio) is greater than 5; By formula weight average and number-average molecular weight are calculated in (1) and (2) respectively:
Mn＝∑MiNi/∑Ni (1)
Mw＝∑Mi 2Ni/∑Ni (2)
Ni is that quality is the content of the ion of Mi in formula (1) and the formula (2).
Described method, wherein, Fourier Transform Ion cyclotron Resonance mass spectrum ionization source is electron spray (ESI).
Described method, wherein, standard specimen and testing sample are to be diluted to 8-10mgml earlier -1Mother liquor, be mixed with 0.1-0.2mgml during mensuration again -1Solution, and add the ammoniacal liquor of 10-15 μ L.
Described method, wherein, the diluting solvent of standard specimen and testing sample is one or more in toluene, tetramethylpyrrolidi-e ketone, tetrahydrofuran and the acetonitrile.
Advantage of the present invention is following:
1) the invention provides the profound method that asphaltene molecule is formed of directly analyzing.
2) core of the present invention is to have set up a standardized method of operating, thereby obtains high-quality spectrogram, has guaranteed the accuracy and the repeatability of spectrogram.
3) the present invention utilizes the characteristic of high resolution mass spectrum ultrahigh resolution and superelevation degree of accuracy, from the different pitch of molecular level identification.
4) use technology of the present invention, can analyze petroleum bitumen, coal-tar pitch, rock asphalt, mix asphalt.
5) the present invention have rapidly, characteristic of accurate.Sample size only needs 10mg.
Description of drawings
Fig. 1 is standard specimen and treats sample high resolution mass spectrum broadband comparison diagram.
Fig. 2 is standard specimen and treats sample high resolution mass spectrum arrowband comparison diagram.
Fig. 3 is standard specimen and the qualitative figure that treats that sample Semi-polarity compound molecule is formed.
Fig. 4 is four kinds of pitch high resolution mass spectrum comparison diagrams.
Fig. 5 is that four kinds of pitches are at the local mass spectrum comparison diagram of m/z=401.
Embodiment
The Fourier Transform Ion cyclotron Resonance mass spectrometer is a kind of novel mass spectrometer with superior quality resolution characteristic, can study petroleum composition from the molecular composition level.Electron spray (ESI) ionization source can be from the complicated hydrocarbon base of high concentration optionally nitrogen, sulphur and the oxygen polar compound of trace in the ionization petroleum component, need not pre-service for petroleum bitumen, overcome the restriction of common gas chromatography mass spectrometry (GC-MS) gasification temperature.Through the Fourier Transform Ion cyclotron Resonance mass spectrum; The molecular composition characteristic of nitrogen, sulphur and oxygen polar compound from molecular level analysis pitch; Because forming, the polar compound of different regions crude production matrix pitch exists than big-difference; Through the molecular difference of contrast pitch Semi-polarity compound, thus the discriminating of realization different pitches.
High resolution mass spectrum has the several data drainage pattern, and different drainage patterns has different application directions.The broadband scanning pattern of high resolution mass spectrum can be obtained the full spectrum of pitch, obtains the molecular composition distributed intelligence of pitch, but the stability of spectrogram can be influenced.And the data stability of arrowband drainage pattern is fine, but molecular composition information is limited.It is the optimum way that addresses the above problem that broadband drainage pattern and arrowband mould collection formula are used in combination, and the molecular composition that both can obtain the full spectrum of pitch distributes, and can obtain the sxemiquantitative data of reliable and stable again.Mass-to-charge ratio is subject to solvent less than 300 spectrogram or impurity disturbs, and mass-to-charge ratio can produce quality greater than 500 spectrogram and discriminates against, and therefore, suitable arrowband acquisition range is between 300-500.The present invention is main analysis means with electron spray Fourier Transform Ion cyclotron Resonance mass spectrum (ESI FT-ICRMS); Detect the molecular composition of pitch Semi-polarity compound, get the weight-average molecular weight and the number-average molecular weight of the data computation pitch in mass-to-charge ratio (m/z) the 150-1000 scope.Choose the data of 20 continuous units in the mass-to-charge ratio 300-500 simultaneously and carry out qualitative and semi-quantitative analysis, and adopt repeated limit method and spectrogram matching method to estimate the difference of sample to be checked and pitch standard specimen, thereby draw identification result.
The pitch of indication of the present invention " fingerprint " information is meant the molecular composition characteristic of heteroatomic polar compounds such as containing nitrogen, sulphur and oxygen in the pitch.Different regions crude oil is widely different; Form by the polar compound of the pitch of different crude production and to have very big difference; The present invention utilizes the Fourier Transform Ion cyclotron Resonance Mass Spectrometer Method to obtain the molecular fingerprint characteristic information of the polar compound under the two kinds of patterns in broadband and arrowband, comprises concrete characteristic informations such as molecular weight and distribution thereof, polar compound type and relative content thereof.The difference of the molecular composition characteristic through contrast pitch Semi-polarity compound, thus realize the discriminating of different pitches.
The present invention can accurately judge kind, the quality of road asphalt and control its quality; Quality to the road asphalt material is effectively supervised; Prevent that the improper of supplier from making profit, make its market standardization, to create good society, economic benefit plays positive role.
Below in conjunction with icon and instance the present invention is described further
Embodiment 1: a kind of discriminating of petroleum bitumen
One, uses instrument
The Apex Ultra of U.S. Bruker company type Fourier Transform Ion cyclotron Resonance mass spectrometer (FT-ICRMS), magnetic field intensity 9.4T, electron spray ionisation source (ESI).
Two, concrete experiment flow.
1) the sample introduction flow velocity that electron spray Fourier Transform Ion cyclotron Resonance mass spectrum (ESI FT-ICR MS) detects pitch being set is 180 μ Lh -1
2) the negative ion detecting pattern of selection electron spray Fourier Transform Ion cyclotron Resonance mass spectrum (ESI FT-ICR MS) is regulated atomization gas flow velocity 1.2Lmin -1, dry gas flow velocity 5Lmin -1, 200 ℃ of dry gas temperature, polarizing voltage 4000V, capillary inlet voltage 4500V, capillary outlet voltage-320V, reflecting plate-300V, quadrupole rod Q1=200Da, radio frequency 700Vpp; Collision energy 1.3V, source storage collection time 0.01s, storage collection time 0.03s, iontophoresis analysis cell flight time 1.2ms; Mass range 150～1000Da is set, sampling number 4M, scanning times 128 times excites decay 12db.
3) the preparation toluene and methanol (1: 3 ,/v: solution 1ml v), add the ammoniacal liquor of 15 μ L, advance blank, spectrogram is noiseless then prepares pitch appearance if detect, otherwise washes until abatement of pollution repeatedly.
4) take by weighing crude oil standard specimen sample introduction calibration instrument, calibration back mass deviation is less than 1ppm.
5) take by weighing pitch 10mg, add 3mL toluene ultrasonic dissolution, arrive 10mgml with dilution with toluene -1, promptly get mother liquor; Get 20 μ L with toluene and methanol (1: 3 ,/v: v) be mixed with 0.2mgml -1, adding the ammoniacal liquor of 15 μ L again, vibration mixes it gently.
6) sampling pump sample introduction when treating that spectrogram is stablized, begins to gather spectrogram, at first selects the broadband scanning pattern, gathers pitch and composes entirely, and spectrogram is gathered 5 times.Be adjusted to the arrowband drainage pattern then, gather the pitch arrowband, spectrogram is gathered 5 times.
7) test sample being done same operation handles
Three, data analysis processing and result thereof
1) 5 groups of data of screening standard specimen and sample to be checked scanning if any the divorce spectrogram, are got rid of this spectrogram, choose two groups of data then and carry out subsequent analysis.
2) choose standard specimen and sample wideband spectrum diagram data to be checked; The screening signal to noise ratio (S/N ratio) is greater than 5 data; Calculate number-average molecular weight and weight-average molecular weight and distribution thereof according to formula (1) and (2), once gathering molecular weight with reference to appearance is Mw/Mn=520/492, is Mw/Mn=520/493 with reference to appearance secondary acquisition molecular weight; It is Mw/Mn=524/494 that sample is once gathered molecular weight, and sample secondary acquisition molecular weight is the Mw/Mn=522/493 (see figure 1).
3) choose standard specimen and sample narrow-band spectrum diagram data (see figure 2) to be checked, retrieval is calculated and is identified main peaks, and main type of compounds is N 1, O 1, O 2, N 1O 2And N 1O 1Heteroatoms type (see figure 3), and choose N 1, O 1, O 2, N 1O 2And N 1O 1This five compounds type is carried out sxemiquantitative and is calculated (result of calculation is seen table 1, table 2).
4) repeated limit method is estimated standard specimen and testing sample molecular weight and all types of relative contents.The computing formula of repeatability limit does
r 95 % = 2 2 S r = 2.8 S r
Sr is a relative standard deviation in the formula
Getting relative standard deviation is 5%, replaces population mean with sample average, then:
r 95 % = 2.8 × x ‾ × 5 % = x ‾ × 14 % ‾
If measure absolute deviation for twice less than r 95%, then both are consistent.
5) comprehensive above the analysis draws analysis result (analysis result is seen table 3).
Embodiment 2: representative petroleum bitumen contrast
According to embodiment 1 methods analyst
Data analysis processing and result thereof
1) 1# molecular weight analyte Mw/Mn=493/465,2# molecular weight analyte Mw/Mn=506/477, # sample molecular weight analyte Mw/Mn=443/414,4# molecular weight analyte Mw/Mn=546/512 (see figure 4).
2) choose the local amplification of m/z=401 in the spectrogram, identify the type of compounds of main peaks, mainly contain N 1, O 1, O 2, O 2S 1And N 2Five kinds of heteroatoms type (see figure 5)s.
3) the spectrogram matching method is estimated four kinds of pitches.No matter at global feature, or local feature, four kinds of pitch significant differences.
Table 1 standard specimen repeatability analysis result
Figure BDA0000102053600000071
Table 2 testing sample repeatability analysis result
Figure BDA0000102053600000072
Table 3 standard specimen and testing sample characteristic index comparative result
Figure BDA0000102053600000073

Claims (8)

1. one kind is utilized the pitch of Fourier Transform Ion cyclotron Resonance mass-spectrometric technique to analyze discrimination method, and its process is:
1) standard specimen is detected in fourier transform ion cyclotron resonance mass spectrometer, measure the mass spectrometric data of wherein polar compound molecular composition and molecular weight and distribution thereof;
2) testing sample is detected in fourier transform ion cyclotron resonance mass spectrometer, measure the mass spectrometric data of wherein polar compound molecular composition and molecular weight and distribution thereof;
3) utilize repeated limit method and spectrogram matching method to estimate the difference of testing sample and standard specimen Semi-polarity compound molecule composition and molecular weight and distribution thereof, thereby obtain identification result.
2. method according to claim 1, wherein, standard specimen and testing sample Semi-polarity compound molecular weight and distribution thereof are under the broadband scanning pattern, the scanning mass-to-charge ratio is the mass spectrometric data in the 150-1000 scope.
3. method according to claim 1 and 2, wherein, standard specimen and testing sample Semi-polarity compound molecular weight and distribution thereof are under the arrowband scan pattern, the scanning mass charge ratio range is the mass spectrometric data in the 440-460 scope.
4. method according to claim 1 and 2 wherein, contains N in standard specimen and the testing sample polar compound 1, O 1, N 1O 1, O 2, N 2, N 1O 2, N 1S 1, O 1S 1, O 2S and N 1O 1S 1Heteroatoms.
5. method according to claim 1, wherein, the molecular weight of standard specimen and testing sample is the mass spectrometric data that is taken under the broadband scanning pattern, and signal to noise ratio (S/N ratio) is greater than 5; By formula weight average and number-average molecular weight are calculated in (1) and (2) respectively:
Mn＝∑MiNi/∑Ni (1)
Mw＝∑Mi 2Ni/∑Ni (2)
Ni is that quality is the content of the ion of Mi in formula (1) and the formula (2).
6. method according to claim 1, wherein, Fourier Transform Ion cyclotron Resonance mass spectrum ionization source is an electron spray.
7. method according to claim 1, wherein, standard specimen and testing sample are to be diluted to 8-10mgml earlier -1Mother liquor, be mixed with 0.1-0.2mgml during mensuration again -1Solution, and add the ammoniacal liquor of 10-15 μ L.
8. method according to claim 7, wherein, the diluting solvent of standard specimen and testing sample is one or more in toluene, tetramethylpyrrolidi-e ketone, tetrahydrofuran and the acetonitrile.
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CN103396818A (en) * 2013-06-25 2013-11-20 交通运输部公路科学研究所 Biological asphalt and its preparation method
CN105987946A (en) * 2015-03-03 2016-10-05 中国石油化工股份有限公司 Oil migration direction tracing method
CN107655783A (en) * 2017-08-30 2018-02-02 江苏诺路桥工程检测有限公司 A kind of detection method for judging mediation hard grades of bitumen
CN110243958A (en) * 2019-05-31 2019-09-17 中国石油天然气股份有限公司 A method of analysis samples for complicated geological component
CN111855789A (en) * 2020-06-12 2020-10-30 交通运输部公路科学研究所 Method for identifying blended asphalt
CN111983006A (en) * 2020-07-31 2020-11-24 河海大学 Method for detecting water loss law of foam warm-mixed asphalt
CN112951345A (en) * 2021-03-10 2021-06-11 中国地质大学（武汉） Method for carrying out oil-reservoir quantitative comparison based on heteroatom compounds
CN113340930A (en) * 2021-05-17 2021-09-03 鞍山钢铁冶金炉材科技有限公司 Method for identifying whether asphalt for converter large-surface feed supplement is adulterated or not by one-step method

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103123330A (en) * 2012-12-19 2013-05-29 长安大学 Method for testing asphalt anti-penetrability performance
CN103396818A (en) * 2013-06-25 2013-11-20 交通运输部公路科学研究所 Biological asphalt and its preparation method
CN105987946A (en) * 2015-03-03 2016-10-05 中国石油化工股份有限公司 Oil migration direction tracing method
CN105987946B (en) * 2015-03-03 2018-12-21 中国石油化工股份有限公司 The tracing method in one oil migration direction
CN107655783A (en) * 2017-08-30 2018-02-02 江苏诺路桥工程检测有限公司 A kind of detection method for judging mediation hard grades of bitumen
CN110243958A (en) * 2019-05-31 2019-09-17 中国石油天然气股份有限公司 A method of analysis samples for complicated geological component
CN111855789A (en) * 2020-06-12 2020-10-30 交通运输部公路科学研究所 Method for identifying blended asphalt
CN111855789B (en) * 2020-06-12 2024-04-09 交通运输部公路科学研究所 Method for identifying blended asphalt
CN111983006A (en) * 2020-07-31 2020-11-24 河海大学 Method for detecting water loss law of foam warm-mixed asphalt
CN111983006B (en) * 2020-07-31 2021-09-28 河海大学 Method for detecting water loss law of foam warm-mixed asphalt
CN112951345A (en) * 2021-03-10 2021-06-11 中国地质大学（武汉） Method for carrying out oil-reservoir quantitative comparison based on heteroatom compounds
CN112951345B (en) * 2021-03-10 2022-06-21 中国地质大学（武汉） Method for carrying out oil-reservoir quantitative comparison based on heteroatom compounds
CN113340930A (en) * 2021-05-17 2021-09-03 鞍山钢铁冶金炉材科技有限公司 Method for identifying whether asphalt for converter large-surface feed supplement is adulterated or not by one-step method

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