CN108490085A - A kind of quick " fingerprint " discriminating detection method for distinguishing lignite - Google Patents
A kind of quick " fingerprint " discriminating detection method for distinguishing lignite Download PDFInfo
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Abstract
The invention discloses a kind of quick " fingerprints " for distinguishing lignite to differentiate detection method, includes the following steps：(1) triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of lignite gas-chromatography/series connection are established：(2) prepare liquid is obtained into full scan total ion current (TIC) chromatographic fingerprinting using the triple level four bars mass spectrograph full scan type collection chromatograms of gas-chromatography/series connection；(3) chromatography " fingerprint " collection of illustrative plates obtained by step (2) and standard " fingerprint " peak figure spectrum obtained by step (1) are compared, sample to be tested is differentiated；(4) sample to be tested that mixed and disorderly, retention time is difficult to differentiate between to " fingerprint " peak peak shape further differentiates sample to be tested using the mass spectrographic SIM patterns of the triple level four bars of gas-chromatography/series connection and MRM Mode scans.This detection method process is easy to operate, analyze speed is fast, can meet the qualitative detection of lignite and other coal classes in coal, also has preferably directiveness to the classification of coal.
Description
Technical field
The present invention relates to a kind of lignite differentiating methods, and in particular to a kind of quick " fingerprint " discriminating detection side for distinguishing lignite
Method.Belong to coal detection technique field.
Background technology
Growing to the demand of the energy with the rapid development of Chinese national economy, the demand to coal is also more
Urgently.Coal is as the important energy and industrial chemicals, and kind determines its value of goods and purposes with classification, in order to ensure reasonable profit
With coal resources, it is necessary to classify to coal.In taxonomic hierarchies, according to indexs such as dry ash free basis volatile matters, by coal
It is divided into the types such as anthracite, bituminous coal and lignite.The differentiation of lignite in recent years is mainly according in coal in China classification national standard
It is distinguished with light transmittance (PM) and gross calorific value on moist ash free basis.
China's standard GB/T/T 2566-2010 at present《The determination of light transmittance method of low rank coal》Middle regulation uses mesh
Depending on the light transmittance of colorimetric method for determining low rank coal, i.e., gained after the mixed liquor of nitric acid and phosphoric acid processing coal sample is used under prescribed conditions
Solution and a series of standard colored solutions colorimetric known to light transmittances, obtain the light transmittance of the solution.This method need to prepare 69 kinds
Standard serial solution is generally available 2~3 months.This method operation is complex, and optical colorimetry is by reviewer's experience etc.
Subjective factor is affected.For PM<30% He>After 90%, it is unable to get specific measured value.It is brown there is an urgent need to more accurately distinguish
The rapid detection method of coal.Discriminating research based on spectrum, chromatography or mass spectrum " finger-print " is it is necessary to attempt or grind
" fingerprint " in the direction studied carefully, domestic literature meaning differentiates, refers generally to naked eyes and compares, but " chromatographic fingerprint " complexity may surpass
Cross the recognizable degree of naked eyes.Discriminant analysis technology based on " chromatographic fingerprint " can make " fingerprint " discriminating become more intuitive and light
Pine.At present " fingerprint " though differentiate apply other materials discriminating have been reported that, the research in terms of lignite discrimination technology is not yet
It appears in the newspapers.
Invention content
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of quick " fingerprint " mirror for distinguishing lignite
Other detection method.The present invention is using acetone as Extraction solvent, with the triple level four bars mass spectrum total ionic chromatographics of gas-chromatography/series connection
Figure (totalions chromatogram, TIC) and mass spectrogram be acquired and analyze, and to sample sample weighting amount, Extraction solvent,
Extraction time, instrument testing conditions etc. are studied, and are provided easy to operate, the qualitative more accurate lignite of one kind and are quickly differentiated
Method.
To achieve the above object, the present invention uses following technical proposals：
A kind of quick " fingerprint " discriminating detection method for distinguishing lignite, includes the following steps：
(1) triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of lignite gas-chromatography/series connection are established：
1. sample pre-treatments：Domestic and international more manufacturers, multiple batches of a variety of coal samples are weighed successively, are placed in centrifuge tube
In, mechanical shaking extraction after organic solvent is vortexed is added, stands, centrifugation takes supernatant, crosses 0.22 μm of organic phase filter membrane, obtains for examination
Product solution；
2. above-mentioned test solution is used the triple level four bars mass spectrograph full scan type collection chromatographies of gas-chromatography/series connection
Figure, obtains coal full scan total ion current (TIC) chromatography " fingerprint " collection of illustrative plates, " is referred to according to full scan total ion current (TIC) chromatography
The lignite characteristic peak occurred in line " collection of illustrative plates is scanned under SIM patterns and MRM patterns, make " fingerprint " peak of lignite obtain into
One step is confirmed, and triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of lignite gas-chromatography/series connection are finally obtained.
(2) by coal sample to be measured, according to step, 1. the sample-pretreating method is handled, and obtains prepare liquid；It will
Prepare liquid obtains full scan total ion current using the triple level four bars mass spectrograph full scan type collection chromatograms of gas-chromatography/series connection
(TIC) chromatographic fingerprinting；
(3) by full scan total ion current (TIC) chromatography " fingerprint " collection of illustrative plates and step of coal sample to be measured obtained by step (2)
(1) triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of gained lignite gas-chromatography/series connection carry out the general character of relative retention time
Comparison, sample to be tested is differentiated；
(4) sample to be tested that mixed and disorderly, retention time is difficult to differentiate between to total ion current (TIC) chromatogram " fingerprint " peak peak shape,
Using the mass spectrographic SIM patterns of the triple level four bars of gas-chromatography/series connection and MRM Mode scans, further reflected to sample to be tested
Not.
Coal scans in total ion current (TIC) chromatogram, and the distinguishing characteristics peak of lignite is at 36.85~37.45min.
Using gas-chromatography connect triple level four bars mass spectrograph full scan type collection chromatograms when, carry out judging characteristic
Peak, and then determine type of coal.Using the mass spectrometry method at scanning feature peak, features described above peak is subjected to further mass spectral analysis,
" fingerprint " peak of lignite is further confirmed.
A variety of coal samples include lignite, anthracite, bituminous coal, coal, other bituminous coal etc..
Preferably, step (1) the sample pre-treatments coal sample sampling amount is 1.000g.
Preferably, the addition ratio 1g of step (1) sample and organic solvent:20mL.
Preferably, the organic solvent is acetone, ethyl acetate, acetonitrile, further preferably acetone.
Preferably, step (1) described vortex time is 1min.
Preferably, step (1) the mechanical shaking extraction time is 60min.
Preferably, step (1) described centrifugal speed is 5000r/min, centrifugation time 5min.
Preferably, above-mentioned chromatography is preferably as condition：
Chromatographic column：Model HP-5MSUI, specification are 30m × 0.25mm × 0.25 μm, fused-silica capillary column；
Carrier gas：High-purity helium, helium purity are 99.999%；
Collision gas：High Purity Nitrogen, purity 99.999%；
Flow velocity：3.8ml/min；
Input mode：Splitless injecting samples；
Column temperature：Using temperature programming, initial 70 DEG C, 2min is kept, then with 25 DEG C/min temperature programmings to 150 DEG C, then
With 3 DEG C/min temperature programmings to 200 DEG C, 8 DEG C/min temperature programmings keep 18min to 280 DEG C；
Injector temperature：280℃；
Sample size：1.0μL；
Mass spectrograph operating condition is preferably：
Ion source：The sources EI；Ion source temperature：300℃；Assist heating temperature：280℃；Solvent delay:5min.
Beneficial effects of the present invention：
After handling sample using the method for the invention, the differentiator in lignite is fully extracted, and use gas-chromatography/
Triple level four bars mass spectrographies of connecting detect the characteristic component in lignite, not only can get the TIC fingerprints for being equivalent to chromatographic fingerprint figure
The advantages of figure, bigger, also resides in, and also object in peak can be determined by the scanning of the mass spectrum result of characteristic peak when retention time is close
Whether matter is consistent, and it is more accurate and reliable that this so that the chromatographic fingerprint of lignite differentiates.
After lignite extract carries out full scan, total ion current figure can quickly detect " fingerprint " peak of lignite, pass through SIM
It is further confirmed at " fingerprint " peak of the characteristic peak of pattern and MRM Mode scans lignite, lignite.This method reduce detection at
This, improves detection efficiency while effectively increasing the accuracy of detection；Detection process is easy to operate simultaneously, analyze speed is fast,
The qualitative detection that lignite and other coal classes in coal can be met also has preferably directiveness to the classification of coal.
Description of the drawings
Fig. 1 is different extracting solution superposition chromatograms；
Fig. 2 difference extracting solution extraction chromatography figures；
Fig. 3 coals scan total ion current (TIC) chromatogram；
Fig. 4 coals scan total ion current (TIC) and are superimposed comparison chromatogram；
Fig. 5 lignite full scan total ion current (TIC) chromatogram；
Fig. 6 lignite selects ion scan (SIM) chromatogram；
Fig. 7 lignite selects ion scan (SIM) mass spectrogram；
Fig. 8 lignite multiple-reaction monitoring pattern (MRM) scans chromatogram；
Reference numeral " HM " is lignite characteristic peak.
Specific implementation mode
The present invention will be further elaborated with reference to the accompanying drawings and examples, it should which explanation, following the description is only
It is not to be defined to its content to explain the present invention.
Embodiment
1. instrument and reagent
The triple level four bars mass spectrographs of gas-chromatography/series connection (Agilent7890A-7000B GC-MS/MS)；Oscillator (moral
State IKAKS260)；Vortex vortex mixer (IKAMS3basic)；Centrifuge (Anting Scientific Instrument Factory, Shanghai).
Ethyl acetate：Chromatographically pure；Acetonitrile：Chromatographically pure；Acetone：Chromatographically pure.
2. instrument operating condition
GC/MS/MS：Chromatographic column：HP-5MSUI (30m × 0.25mm i.d., 0.25 μm) fused-silica capillary column；It carries
Gas：High-purity helium (99.999%)；Collision gas：High Purity Nitrogen (99.999%)；Flow velocity：3.8ml/min；Input mode：It does not shunt
Sample introduction；Column temperature：Initial 70 DEG C (2min) with 25 DEG C/min temperature programmings to 150 DEG C, then with 3 DEG C/min temperature programmings to 200 DEG C,
8 DEG C/min temperature programmings keep 18min to 280 DEG C；Injector temperature:280℃；1.0 μ L of sample size；Ion source：The sources EI；From
Source temperature：300℃；Assist heating temperature：280℃；Solvent delay:5min.
3. sample pre-treatments
1.000g coal samples are weighed, are placed in 50mL centrifuge tubes, mechanical shaking extraction after 20mL acetone vortexs 1min is added
60min stands 5min, centrifuges 5min with 5000r/min, takes supernatant 1mL, and machine in 0.22 μm of organic phase filter membrane of crossing measures.
(1) selection of sample weighting amount
0.200g, 0.500g, 0.800g, 1.000g, 1.500g are weighed respectively, and 20mL acetone whirlpool is added in 2.000g samples
Machine measures on centrifuging and taking supernatant after rotation, mechanical shaking extraction.0.200g, 0.500g sample instrumental response value are relatively small, 2.0g samples
Capo load excessive, peak shape are undesirable.It is screened through test of many times, 0.800g, 1.000g, sample size peak shape and the response of 1.500g
Value is preferable, and sample size peak shape and the response of wherein 1.000g are best.
(2) selection of Extraction solvent
1.000g lignite samples are weighed successively, are separately added into 20mL acetone, ethyl acetate, acetonitrile, and vortex 1min, oscillation carry
Take 60min, the color of lignite extracting solution is dark brown after acetone extraction, and the color of lignite extracting solution is shallow brown after acetonitrile extraction
Color, using the triple level four bars mass spectrograph full scan type collection chromatograms of gas-chromatography series connection, different extracting solutions are superimposed chromatograms
As shown in Figure 1, numeral mark is respectively " 1 "-acetone extract in figure；" 2 "-acetic acid ethyl acetate extract；" 3 "-acetonitrile extracting solution
Chromatogram.Different extracting solution extraction chromatography figures are as shown in Fig. 2, numeral mark is respectively " 1 "-acetone extract in figure；“2”-
Acetic acid ethyl acetate extract；The chromatogram of " 3 "-acetonitrile extracting solution.
As can be seen that acetone extract response highest, peak shape are best from acquisition chromatogram, extraction effect is most ideal.Second
Chromatography peak response is low, peak shape is poor after acetoacetic ester, the extraction of acetonitrile extracting solution, and enters gas chromatographic column after acetonitrile solution sample introduction to color
Spectrum column damages.
Anthracite, coal, other bituminous coal and bituminous coal sample are weighed successively, acetone, ethyl acetate, acetonitrile is added, be vortexed
1min, mechanical shaking extraction 60min, experiment find extraction effect with lignite extraction effect, acetone extraction solution in three kinds of Extraction solvents
Chromatography response is high, peak shape is good, final to determine that acetone is that lignite extracts most by the extraction effect of Experimental Comparison different solvents
Good Extraction solvent.
(3) selection of extraction time
After Extraction solvent is added in sample, extracting solution color is constantly deepened, and per 10min examination with computer responses, is carried after 60min
Take liquid color keep constant, response is not also further added by.Experiment is final to determine that extraction time is 60min.
(4) selection of instrument condition
Coal extract is natural goods, and containing there are many small molecule hydrocarbon class, gas-chromatography/series connection three is utilized after sample is extracted
The mass spectrograph detection of weight level four bars, experiment accelerate the appearance of small molecule hydro carbons, while utilizing solvent delay by increase column flow,
Small molecule peak is filtered.And then temperature programming is used, improve the separating degree of sample to be tested.Lignite is because containing the changes such as macromolecular phenols
Object is closed, therefore extracting solution color is brown, constantly deepens with the color that increases of content of phenolic hydroxyl groups, but macromolecular compound molecule
Amount is big, boiling point high appearance evening in chromatogram, thus is removed micromolecular compound by optimizing chromatographic condition, after mass spectrum acquisition
There is target peak, which is feature macromolecular compound chromatographic peak in lignite, and such compound is lignite characteristic compounds.
By scanning this feature compound, " fingerprint " peak of lignite is obtained, so as to quickly distinguish lignite.
4. quick " fingerprint " of distinguishing lignite differentiates detection method and its result verification
Lignite, anthracite, coal, other bituminous coal and bituminous coal the sample upper machine testing after 1.3 pre-treatments, in full scan pattern
Obtained chromatogram is as shown in Figure 3 and Figure 4, and number is respectively 1- lignite in figure；2- anthracites；3- coals；The other bituminous coal of 4-；5-
Bituminous coal；" HM " is labeled as the characteristic peak of lignite in Fig. 4.
It will be seen that more batches of lignite samples, lignite utilize gas after acetone extraction both at home and abroad by detection from Fig. 5
The triple level four bars mass spectrograph full scan patterns of phase chromatography/series connection carry out full scan, and wherein lignite occurs in 36.85~37.45min
One characteristic peak, other type coals are free of the compound.Confirm that the chromatographic peak is lignite feature " fingerprint " peak from TIC figures
On, lignite and other type coals can be distinguished by " fingerprint " peak in lignite chromatogram, is retrieved from the libraries NISST
The compound is macromolecular phenolic compound, but needs this differentiation of more experimental results confirmations.
Chromatographic signal sampling is carried out to the lignite sample of different batches different location using the above method and establishes gas-chromatography
Standard finger-print, gas chromatography standard finger-print test result are as follows：
1 Shaanxi lignite TIC figure retention time results of table
2 Heilungkiang lignite TIC figure retention time results of table
3 Indonesia's lignite TIC figure retention time results of table
The Russian lignite TIC figure retention time results of table 4
By carrying out multiple data acquisition, reservation of each sample in same batch sample introduction to different sources different batches sample
Time indifference, the place of production is identical, the difference of the retention time between different batches sample, but the variation of its retention time is little.
Chromatographic condition and chromatography column condition are not fully identical when because of every batch of sample feeding, and the variation of retention time is normal change
Change.Domestic and international lignite sample characteristic peak retention time no significant difference, every batch of sample are can be seen that by data comparison in table
It is reproducible.
Since chromatographic fingerprint comparison is mainly by features such as the combination forms at the presence or absence of peak, height and several peaks.Chromatography point
Easily there is shift of retention time phenomenon in analysis, and it is qualitative by retention time when, substance also differs in the identical peak of retention time
Surely it is same or same group of compound.The triple level four bars mass spectrographs of gas-chromatography/series connection are in analyzing lignite TIC chromatograms
While (Fig. 5) feature " fingerprint " peak, the mass spectrometry method at scanning feature peak may be used, to judge the component of substance in peak, this
This feature peak is carried out further mass spectral analysis by experiment, selected in the case where selecting ion scan (SIM) pattern ion mass-to-charge ratio for：
190.8,167.8,144.8,280.7 are scanned, and scan chromatogram and mass spectrogram as shown in Fig. 6~Fig. 7.
Lignite feature " fingerprint " peak quilt is can be seen that by lignite full scan ion figure and selection ion scan chromatogram
Further separation selects ion scan pattern more acurrate can obtain feature in lignite " fingerprint " peak, can be more acurrate by lignite
It is distinguished with other type coals.
Further to confirm to feature in lignite " fingerprint " peak, by lignite extracting solution in multiple-reaction monitoring pattern
(MRM) it is scanned under pattern, feature parent ion selection 394.8, ion pair is 394.8/187 collision energy 25, ion pair
For 394.8/95 collision energy 25, ion pair is 394.8/161 collision energy 25, and ion pair is 394.8/159.1 collision energies
30, it scans chromatogram and mass spectrogram is as shown in Figure 8.
It can be seen by chromatogram under lignite full scan ion figure, selection ion scan chromatogram and multiple-reaction monitoring pattern
Go out, which is completely segregated, and lignite characteristic component compound " fingerprint " peak is bright
Aobvious, lignite feature " fingerprint " peak is identified, under the scan pattern that lignite and other coals is quick, accurately distinguish.
Mass spectrum fingerprint is more complicated than chromatographic fingerprint, and data information amount is big, but hiding rule is also more, to the qualitative of compound
It is more accurate.After carrying out full scan to lignite, total ion current figure can quickly detect " fingerprint " peak of lignite, be swept by SIM
It retouches, characteristic compounds are obviously distinguished by its characteristic peak in lignite, and " fingerprint " peak of lignite definitely, further passes through
MRM Mode scans can be clearly seen that " fingerprint " peak of lignite, so as to " fingerprint " confirmed from chromatogram
Peak.Sample is detected after acetone extraction using the triple level four bars mass spectrographs of gas-chromatography/series connection, under full scan pattern
To " fingerprint " peak of lignite, " fingerprint " peak of lignite is further confirmed under SIM patterns and MRM patterns.
The coal sample of different sources different batches is carried out using the above method to verify its gas-chromatography/series connection triple four
Grade bar mass spectrum " fingerprint " collection of illustrative plates, test result are as follows：
6 all kinds of coal TIC of table scheme Experimental comparison results
Coal all over the world is compared according to experimental result, all kinds of coal contrast tables are as follows：
7 all kinds of coal TIC of table scheme Experimental comparison results
| Serial number | Inspection declaration coal classification | The place of production | Volatile matter Vdef, % | Fixed carbon content F Cdef, % | Characteristic peak |
| 1. | Lignite | It is domestic | 40~60 | ≤60 | Have |
| 2. | Lignite | It is external | 40~60 | ≤60 | Have |
| 3 | Anthracite | It is domestic | <10 | >90 | Nothing |
| 4 | Anthracite | It is external | <10 | >90 | Nothing |
| 5 | Injection coal | It is domestic | <10 | - | Nothing |
| 6 | Injection coal | It is external | <10 | - | Nothing |
| 7 | Other bituminous coal | It is domestic | 10~50 | 50~90 | Nothing |
| 8 | Other bituminous coal | It is external | 10~50 | 50~90 | Nothing |
| 9 | Coal | It is domestic | 70 | - | Nothing |
| 10 | Coal | It is external | 70 | - | Nothing |
This research method is found by detecting a variety of coal samples both at home and abroad, using the triple level four bars of gas-chromatography/series connection
Mass spectrography detects the differentiation that the method that lignite is distinguished at " fingerprint " peak in the characteristic component in lignite is suitable for various countries' lignite, the party
Method reduces testing cost, improves detection efficiency while effectively increasing the accuracy of detection.Detection process is easy to operate, divides
It is fast to analyse speed, the qualitative detection of lignite and other coal classes in coal can be met, also there is preferably guidance to anticipate the classification of coal
Justice.
After handling sample using methods described herein, the differentiator in lignite is fully extracted, and utilizes gas-chromatography/series connection
Characteristic component in triple level four bars mass spectrography detection lignite, not only can get the TIC fingerprint images for being equivalent to chromatographic fingerprint figure,
The advantages of bigger, also resides in, and can also determine in peak whether is substance by the scanning of the mass spectrum result of characteristic peak when retention time is close
Unanimously, it is more accurate and reliable so that the chromatographic fingerprint of lignite differentiates for this.
After lignite extract carries out full scan, total ion current figure can quickly detect " fingerprint " peak of lignite, pass through SIM
It is further confirmed at " fingerprint " peak of the characteristic peak of pattern and MRM Mode scans lignite, lignite.This method and traditional lignite area
Divide method to compare easy to operate, quick, reduces testing cost without preparing multiple standards solution, improve detection efficiency, adopt
It is detected with the triple level four bars mass spectrographs of gas-chromatography/series connection and effectively increases detection compared with traditional visual colorimetric determination spectrometry
Accuracy.This method detection process is easy to operate, analyze speed is fast, it is reproducible, qualitative can accurately meet in coal lignite with
The qualitative detection that other type coals are distinguished also has preferably directiveness to the classification of coal.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, based on the technical solutions of the present invention, those skilled in the art, which need not make the creative labor, to be done
The various modifications or changes gone out are still within protection scope of the present invention.
Claims (8)
1. a kind of quick " fingerprint " for distinguishing lignite differentiates detection method, which is characterized in that include the following steps：
(1) triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of lignite gas-chromatography/series connection are established：
1. sample pre-treatments：Domestic and international more manufacturers, multiple batches of a variety of coal samples are weighed successively, are placed in centrifuge tube,
Mechanical shaking extraction after organic solvent is vortexed is added, stands, centrifugation takes supernatant, crosses 0.22 μm of organic phase filter membrane, it is molten to obtain test sample
Liquid；
2. above-mentioned test solution is used into the triple level four bars mass spectrograph full scan type collection chromatograms of gas-chromatography/series connection,
Coal full scan total ion current (TIC) chromatography " fingerprint " collection of illustrative plates is obtained, according to full scan total ion current (TIC) chromatography " fingerprint " figure
The lignite characteristic peak occurred in spectrum is scanned under SIM patterns and MRM patterns, and " fingerprint " peak of lignite is made to obtain further
Confirmation finally obtains triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of lignite gas-chromatography/series connection.
(2) by coal sample to be measured, according to step, 1. the sample-pretreating method is handled, and obtains prepare liquid；It will be to be measured
Liquid obtains full scan total ion current using the triple level four bars mass spectrograph full scan type collection chromatograms of gas-chromatography/series connection
(TIC) chromatographic fingerprinting；
(3) by full scan total ion current (TIC) chromatography " fingerprint " collection of illustrative plates of coal sample to be measured obtained by step (2) and step (1)
Triple level four bars mass spectrum standard " fingerprint " the peak figure spectrums of gained lignite gas-chromatography/series connection carry out the ratio of the general character of relative retention time
Compared with differentiating to sample to be tested；
(4) sample to be tested that mixed and disorderly, retention time is difficult to differentiate between to total ion current (TIC) chromatogram " fingerprint " peak peak shape uses
The mass spectrographic SIM patterns of the triple level four bars of gas-chromatography/series connection and MRM Mode scans, further differentiate sample to be tested.
2. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that described
Chromatographic condition is：
Chromatographic column：Model HP-5MSUI, specification are 30m × 0.25mm × 0.25 μm, fused-silica capillary column；
Carrier gas：High-purity helium, helium purity are 99.999%；
Collision gas：High Purity Nitrogen, purity 99.999%；
Flow velocity：3.8ml/min；
Input mode：Splitless injecting samples；
Column temperature：Using temperature programming, initial 70 DEG C, 2min is kept, then with 25 DEG C/min temperature programmings to 150 DEG C, then with 3
DEG C/min temperature programmings to 200 DEG C, 8 DEG C/min temperature programmings keep 18min to 280 DEG C；
Injector temperature：280℃；
Sample size：1.0μL.
3. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that
The Mass Spectrometry Conditions are：Ion source：The sources EI；Ion source temperature：300℃；Assist heating temperature：280℃；Solvent delay:
5min。
4. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that step
(1) addition of the sample and organic solvent ratio 1g:20mL.
5. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that described
Organic solvent is acetone, ethyl acetate, acetonitrile, further preferably acetone.
6. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that step
(1) the mechanical shaking extraction time is 60min.
7. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that
Step (1) described vortex time is 1min.
8. a kind of quick " fingerprint " for distinguishing lignite according to claim 1 differentiates detection method, which is characterized in that
Step (1) described centrifugal speed is 5000r/min, centrifugation time 5min.
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| CN114577966A (en) * | 2020-11-18 | 2022-06-03 | 湘潭大学 | GC x GC fingerprint fast comparison method for classification of MSCC combined with modulation peak |
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| CN114577966A (en) * | 2020-11-18 | 2022-06-03 | 湘潭大学 | GC x GC fingerprint fast comparison method for classification of MSCC combined with modulation peak |
| CN114577966B (en) * | 2020-11-18 | 2023-08-08 | 湘潭大学 | GC x GC fingerprint rapid comparison method for classifying MSCC combined with modulation peak |
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| CN108490085B (en) | 2021-01-22 |
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